CN114657365B - Pure titanium sheet with surface crystal patterns and processing method thereof - Google Patents
Pure titanium sheet with surface crystal patterns and processing method thereof Download PDFInfo
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- CN114657365B CN114657365B CN202210367037.2A CN202210367037A CN114657365B CN 114657365 B CN114657365 B CN 114657365B CN 202210367037 A CN202210367037 A CN 202210367037A CN 114657365 B CN114657365 B CN 114657365B
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- 239000010936 titanium Substances 0.000 title claims abstract description 139
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 133
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 239000013078 crystal Substances 0.000 title claims abstract description 90
- 238000003672 processing method Methods 0.000 title description 9
- 238000000034 method Methods 0.000 claims abstract description 35
- 230000008569 process Effects 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims description 39
- 238000004321 preservation Methods 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 26
- 238000010791 quenching Methods 0.000 claims description 18
- 230000000171 quenching effect Effects 0.000 claims description 18
- 238000005202 decontamination Methods 0.000 claims description 10
- 230000003588 decontaminative effect Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims description 8
- 239000002932 luster Substances 0.000 claims description 7
- 230000009466 transformation Effects 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910000734 martensite Inorganic materials 0.000 claims description 4
- 238000000265 homogenisation Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 230000003373 anti-fouling effect Effects 0.000 abstract description 6
- 235000017060 Arachis glabrata Nutrition 0.000 abstract description 4
- 241001553178 Arachis glabrata Species 0.000 abstract description 4
- 235000010777 Arachis hypogaea Nutrition 0.000 abstract description 4
- 235000018262 Arachis monticola Nutrition 0.000 abstract description 4
- 235000020232 peanut Nutrition 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 229910052786 argon Inorganic materials 0.000 description 8
- 239000000243 solution Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000009966 trimming Methods 0.000 description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000034655 secondary growth Effects 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D11/00—Process control or regulation for heat treatments
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D11/00—Process control or regulation for heat treatments
- C21D11/005—Process control or regulation for heat treatments for cooling
-
- 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
-
- 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
-
- 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
Abstract
The invention provides a pure titanium plate, which is a pure titanium plate with a scaly crystal flower apparent structure on the surface; the size of the scaly crystal flower is more than 3mm and less than or equal to 8mm. The pure titanium sheet has scaly crystal flowers with specific sizes, and the crystal flowers have uniform sizes and standard shapes. The surface of the crystal flower has the characteristics of high smoothness, strong anti-fouling capability, no blackening of the surface for a long time and strong oxidation resistance. After the processing of the invention, the crystal structure of the metal on the surface of the titanium sheet is unchanged, and the titanium sheet is low-temperature stable phase alpha-Ti. In addition, the pore diameter of the micropores on the surface of the titanium material is smaller, the number of the micropores is reduced, and the structure is more compact after the titanium material is processed by the process. The preparation method provided by the invention has the characteristics of simple process, low processing cost, high peanut forming speed, uniform size of the crystal flower, easiness in operation and the like, and can be applied to a large-scale industrial production line.
Description
Technical Field
The invention belongs to the technical field of heat treatment of the surface of a pure titanium sheet, relates to a pure titanium sheet and a preparation method thereof, and particularly relates to a pure titanium sheet with surface crystal patterns and a processing method thereof.
Background
The surface of the pure titanium sheet metal is the natural color of metal, the appearance is too single, the application of the titanium sheet metal product is greatly limited, and along with the increasing demands of consumers on titanium products, the surface of the titanium product is also in urgent need of diversification. In addition, titanium products of metallic natural color have the defect of blackening along with surface oxidation. The crystal flower treatment on the surface of the titanium thin plate not only can make the titanium product more beautiful, but also can overcome the defect of blackening on the surface of the titanium product.
Some improved schemes are also disclosed in the prior art, such as a preparation method of needle crystal patterns of titanium products, but the preparation method is complex, a heating and heat preservation process is needed to be carried out in three stages, the treatment process efficiency is low, the three processing time consumption is 16 hours, at least 3.75 hours is needed, the energy consumption is high, and the environment is not protected. The technical proposal also discloses a processing method of the crystal patterns of the titanium product, but in the preparation process, the temperature is directly raised to more than 1000 ℃ to cause the overquick growth speed of the crystal, and the grain size distribution and the shape uniformity of the crystal grains can not be effectively controlled; particularly, the thin-wall product formed by cold working consumes more energy due to the release of local cold working stress and the recrystallization of broken grains, and has obvious difference from other patterns in size and shape. The diffusion speed of oxygen element under high temperature (above 1000 ℃) is larger than the generation speed of oxide film, and the surface of the material can keep metallic luster without oxidation. In addition, the process needs to be added with high pollution procedures such as polishing, acid washing etching and the like after the heat treatment of the process, so that the metallic luster can be obtained. For thin-wall parts with the thickness of less than 0.8mm, particularly for the parts with complex shapes, the polishing process can not be almost completed, and the acid washing etching is uneven.
Therefore, how to find a more suitable preparation process of crystal flowers on the surface of the pure titanium sheet material, which solves the technical problems, and is especially suitable for the pure titanium sheet material, becomes one of the problems to be solved by domestic research and development type production enterprises and first-line researchers.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a pure titanium sheet material and a preparation method thereof, especially a pure titanium sheet material with surface crystal patterns. The pure titanium sheet provided by the invention has the scaly crystal flowers with specific sizes, the crystal flowers are uniform in size, and the crystal flower surface has the characteristics of high smoothness, strong anti-fouling capability, no blackening on the surface for a long time and strong oxidation resistance. Meanwhile, the preparation process is simple, the processing cost is low, the peanut forming speed is high, the operation is easy, and the method is more suitable for popularization and application of industrial mass production.
The invention provides a pure titanium plate, which is a pure titanium plate with a scaly crystal flower apparent structure on the surface;
the size of the scaly crystal flower is more than 3mm and less than or equal to 8mm.
Preferably, the pure titanium plate is a pure titanium thin plate;
the thickness of the pure titanium plate is 0.4-2 mm;
the purity of the pure titanium plate is more than or equal to 99.6 percent of Ti.
Preferably, the flaky crystal flower is specifically a flaky crystal flower formed by martensitic transformation;
the scaly crystal flowers are scaly crystal flowers with metallic luster;
the scaly crystal flowers are uniformly distributed scaly crystal flowers.
Preferably, the scaly crystal flowers are quenched and cooled to the phase transition temperature T in the pure titanium plate β The following steps were carried out;
before quenching and cooling, the pure titanium plate is subjected to two-step heat treatment;
the shape and/or size of the scaly crystal flower is adjusted by controlling the technological parameters of heat treatment and the quenching speed;
the roughness of the surface of the pure titanium plate is 0.3-0.6 mu m.
The invention also provides a preparation method of the pure titanium plate, which comprises the following steps:
1) Under the vacuum condition, after the first temperature rise and heat preservation step and the second temperature rise and heat preservation step, the pure titanium sheet material is subjected to rapid air cooling quenching treatment, and then the pure titanium sheet material with the scaly crystal flower apparent structure on the surface is obtained;
the heat preservation time of the second heating and heat preservation is more than 2.5 hours and less than or equal to 3.5 hours.
Preferably, the pure titanium sheet material comprises pure titanium sheet or pure titanium sheet product;
the pure titanium thin plate raw material is a pretreated pure titanium thin plate raw material;
the pretreatment includes a buffing and/or decontamination step.
Preferably, the degree of polishing is a mirror surface;
the roughness after the grinding and polishing is 0.3-0.6 mu m;
the decontamination mode comprises the steps of cleaning decontamination under ultrasonic waves by adopting alkali solution.
Preferably, the vacuum pressure is 5.0X10 or less -3 Pa；
The temperature rising rate of the first temperature rising and heat preserving is 5-30 ℃/s;
the temperature of the first heating and heat preservation is 550-650 ℃;
the heat preservation time of the first heating and heat preservation is 1-3 h;
the first heating and heat preserving step is a grain homogenization process.
Preferably, the temperature rising rate of the second temperature rising and preserving is 5-30 ℃/s;
the heat preservation temperature of the second heating and heat preservation is T β ～950℃；
The T is β Is 833-890 ℃;
the second heating and heat preserving step is a crystal grain regrowth process.
Preferably, the rapid air cooling is specifically performed by adopting inert gas;
the pressure of the inert gas for rapid air cooling is 0.05-0.15 MPa;
the cooling rate of the rapid air-cooling quenching treatment is 5-15 ℃/s;
the cut-off temperature of the rapid air-cooled quenching is T β Temperature or lower.
The invention provides a pure titanium plate, which is a pure titanium plate with a scaly crystal flower apparent structure on the surface; the size of the scaly crystal flower is more than 3mm and less than or equal to 8mm. Compared with the prior art, the pure titanium thin plate provided by the invention has scaly crystal flowers with specific sizes, and the crystal flowers are uniform in size and standard in shape. The surface of the crystal flower has the characteristics of high smoothness, strong anti-fouling capability, no blackening of the surface for a long time and strong oxidation resistance.
The invention also provides a processing method of the crystal flower on the surface of the pure titanium thin plate, the titanium thin plate obtains a uniform flaky crystal flower surface treatment process on the surface of a titanium thin plate product by controlling the twice heating process and the heat preservation time and controlling the cooling speed of the titanium thin plate in a vacuum environment, and the obtained crystal flower surface has the characteristics of high smoothness, uniform crystal flower size, strong anti-fouling capability, no blackening of the surface for a long time and strong oxidation resistance. After the processing of the invention, the crystal structure of the metal on the surface of the titanium sheet is unchanged, and the titanium sheet is low-temperature stable phase alpha-Ti. In addition, the pore diameter of the micropores on the surface of the titanium material is smaller, the number of the micropores is reduced, and the structure is more compact after the titanium material is processed by the process.
The preparation method provided by the invention has the characteristics of simple process, low processing cost, high peanut forming speed, uniform size of the crystal flower, easiness in operation and the like, and can be applied to a large-scale industrial production line.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention and are not limiting of the invention claims.
All the raw materials of the present invention are not particularly limited in their sources, and may be purchased on the market or prepared according to conventional methods well known to those skilled in the art.
The purity of all the raw materials of the invention is not particularly limited, and the invention preferably adopts the conventional purity requirement in the field of preparing industrial pure or pure titanium plates.
All raw materials of the invention, the brands and abbreviations of which belong to the conventional brands and abbreviations in the field of the related application are clear and definite, and the person skilled in the art can purchase from the market or prepare by the conventional method according to the brands, abbreviations and the corresponding application.
The process used in the invention, the abbreviations thereof belong to the conventional abbreviations in the field, the specific steps and the conventional parameters of each abbreviation are clear and definite in the related field, and the process can be realized by a conventional method according to the abbreviations by a person skilled in the art.
The invention provides a pure titanium plate which is of a scale-shaped crystal flower apparent structure on the surface.
The size of the scaly crystal flower is more than 3mm and less than or equal to 8mm.
In the present invention, the size of the flaky crystalline flower is preferably 3 to 8mm, more preferably 4 to 7mm, and still more preferably 5 to 6mm.
In the present invention, the pure titanium sheet is preferably a pure titanium thin sheet.
In the present invention, the thickness of the pure titanium plate is preferably 0.4 to 2mm, more preferably 0.7 to 1.7mm, and still more preferably 1.0 to 1.4mm.
In the invention, the purity of the pure titanium plate is preferably more than or equal to 99.6 percent of Ti, more preferably more than or equal to 99.7 percent of Ti, and even more preferably more than or equal to 99.8 percent of Ti.
In the present invention, the flaky crystal flower is particularly preferably a flaky crystal flower formed by martensitic transformation.
In the present invention, the flaky crystal flowers are preferably flaky crystal flowers having metallic luster.
In the present invention, the flaky crystal flowers are preferably uniformly distributed flaky crystal flowers.
In the invention, the flaky crystal patterns are preferably cooled to the phase transition temperature T in the quenching of the pure titanium plate β The following results were obtained. Wherein, in the invention, the phase transition temperature T β I.e. the concept of the phase transition temperature of pure titanium, which is well known to the person skilled in the art. Specifically T β The transformation temperature of the alpha-beta phase of the pure titanium metal can be 833-890 ℃ according to the influence factors of heating temperature, heating speed, cooling speed, different batches and the like.
In the invention, the pure titanium plate material is preferably subjected to two-step heat treatment before quenching and cooling.
In the present invention, the morphology and/or size of the scaly flowers is preferably adjusted by controlling the process parameters of the heat treatment and the rate of quenching.
In the present invention, the roughness of the pure titanium plate surface is preferably 0.3 to 0.6. Mu.m, more preferably 0.35 to 0.55. Mu.m, still more preferably 0.4 to 0.5. Mu.m.
The invention provides a preparation method of a pure titanium plate, which comprises the following steps:
1) Under the vacuum condition, the pure titanium sheet material is subjected to a first heating and heat preservation step and a second heating and heat preservation step, and then is subjected to rapid air cooling quenching treatment, so that the pure titanium sheet material with the scaly crystal flower apparent structure on the surface is obtained.
In the present invention, the second temperature rise and holding time is more than 2.5 hours and not more than 3.5 hours, more preferably not less than 2.7 hours and not more than 3.3 hours, still more preferably not less than 2.9 hours and not more than 3.1 hours.
In the present invention, the pure titanium sheet raw material preferably includes a pure titanium sheet or a pure titanium sheet product.
In the present invention, the pure titanium sheet raw material is preferably a pretreated pure titanium sheet raw material.
In the present invention, the pretreatment preferably includes a buffing and/or decontamination step, more preferably a buffing and decontamination step.
In the present invention, the degree of the lapping is preferably a mirror surface.
In the present invention, the roughness after the lapping and polishing is preferably 0.3 to 0.6. Mu.m, more preferably 0.35 to 0.55. Mu.m, still more preferably 0.4 to 0.5. Mu.m.
In the present invention, the means for decontamination preferably includes washing decontamination with an alkali solution under ultrasonic waves.
In the present invention, the pressure of the vacuum is preferably 5.0X10 or less -3 Pa。
In the present invention, the temperature rise rate of the first temperature rise and heat preservation is preferably 5 to 30℃per second, more preferably 10 to 25℃per second, and still more preferably 15 to 20℃per second.
In the present invention, the first temperature rise and holding is preferably 550 to 650 ℃, more preferably 570 to 630 ℃, and even more preferably 590 to 610 ℃.
In the present invention, the first temperature rise and holding time is preferably 1 to 3 hours, more preferably 1.4 to 2.6 hours, and still more preferably 1.8 to 2.2 hours.
In the present invention, the first temperature raising and maintaining step is preferably a grain homogenization process.
In the present invention, the temperature rise rate of the second temperature rise and heat preservation is preferably 5 to 30℃per second, more preferably 10 to 25℃per second, and still more preferably 15 to 20℃per second.
In the invention, the heat preservation temperature of the second heating and heat preservation is preferably T β About 950 ℃, more preferably T β About 930 ℃, more preferably T β ～910℃。
In the present invention, the T β Preferably 833 to 890 ℃, more preferably 843 to 880 ℃, and even more preferably 853 to 870 ℃.
In the present invention, the second temperature raising and maintaining step is preferably a grain regrowth process.
In the present invention, the rapid air cooling is particularly preferably performed by using an inert gas.
In the present invention, the inert gas pressure of the rapid air cooling is preferably 0.05 to 0.15MPa, more preferably 0.07 to 0.13MPa, and still more preferably 0.09 to 0.11MPa.
In the present invention, the cooling rate of the rapid air-cooling quenching treatment is preferably 5 to 15 ℃/s, more preferably 7 to 13 ℃/s, and still more preferably 9 to 11 ℃/s.
In the invention, the cut-off temperature of the rapid air-cooled quenching is preferably T β Temperature or lower.
In the present invention, the T β Preferably 833 to 890 ℃, more preferably 843 to 880 ℃, and even more preferably 853 to 870 ℃.
The invention is a better complete and refined integral processing method, which ensures the uniformity and size uniformity of flaky crystal patterns on the surface of a pure titanium sheet, and better improves the apparent characteristics and sheet properties of the pure titanium sheet, and the preparation method of the pure titanium sheet specifically comprises the following steps:
the invention provides a processing method of crystal flowers on the surface of a pure titanium thin plate (Ti is more than or equal to 99.6 percent and the thickness is 0.4 mm-2 mm), which comprises the following steps:
a. polishing: polishing the surface of the titanium thin plate or the titanium plate product to a mirror surface with the roughness of 0.3-0.6 mu m;
b. degreasing: cleaning greasy dirt remained on the surface by using alkali solution, and drying by cold air for standby after cleaning;
c. heat treatment environment: placing the cleaned and blow-dried titanium sheet or titanium sheet product in a vacuum heating furnace, wherein the air pressure in the furnace is 5.0 multiplied by 10 -3 Pa or below.
d. Homogenizing crystal grains: heating up for the first time, heating up a titanium thin plate or a titanium plate product to 550-650 ℃ in a vacuum heating furnace, and preserving heat for 2h;
e. the grains grow again: continuously heating to T β The temperature is kept at 950 ℃ for more than 2.5 hours and less than or equal to 3.5 hours;
f. quenching: after heat preservation, argon is introduced to cool to the phase transition temperature T β Continuing air cooling to 80-100 ℃ and taking out.
Specifically, the washing in the step b is to wash with an alkali solution under ultrasonic waves, and then wash with flowing distilled water.
Specifically, the air pressure in the vacuum furnace in the step c can be 5.0X10 -3 Pa, more preferably 2.0X10 -3 The vacuum effect of Pa is better.
Specifically, the heating rate of the vacuum furnace in the step d is 5-30 ℃/s, the volume size of the titanium metal crystals can be homogenized in the process, and a structure with the same size is obtained, so that preparation is made for the next reaction.
Specifically, T is as described in step e β The transformation temperature of alpha-beta phase of pure titanium is 833-890 ℃ according to the influence factors of heating temperature, heating speed, cooling speed, different batches and the like, the surface microscopic atomic rearrangement phenomenon of pure titanium metal crystals occurs in the secondary growth process, and as the size and volume of the crystals grow up, the surface fine defects are eliminated.
Specifically, the air pressure of the introduced argon gas in the step f is 0.05-0.15 MPa, the cooling speed is relatively gentle, the titanium metal is subjected to martensitic transformation through a transformation zone, scale-shaped crystal flowers are formed on the surface of the titanium metal, the size of the scale-shaped crystal flowers is 3.0-8.0 mm, and the scale-shaped crystal flowers are uniform in size and can be stored; different air pressures can lead the titanium metal to obtain different cooling speeds, so that the secondary heat preservation temperature can be adjusted accordingly.
The invention provides a pure titanium sheet with surface crystal flowers and a processing method thereof, and the pure titanium sheet prepared by the invention has scale-shaped crystal flowers with specific sizes, uniform crystal flower sizes and standard shapes. The surface of the crystal flower has the characteristics of high smoothness, strong anti-fouling capability, no blackening of the surface for a long time and strong oxidation resistance.
According to the processing method of the crystal flowers on the surface of the pure titanium thin plate, provided by the invention, the titanium thin plate is subjected to a surface treatment process of uniform flaky crystal flowers on the surface of a titanium thin plate product by controlling the twice heating process and the heat preservation time and controlling the cooling speed of the titanium thin plate in a vacuum environment, and the obtained crystal flower surface has the characteristics of high smoothness, uniform crystal flower size, strong anti-fouling capability, no blackening of the surface for a long time and strong oxidation resistance. After the processing of the invention, the crystal structure of the metal on the surface of the titanium sheet is unchanged, and the titanium sheet is low-temperature stable phase alpha-Ti. In addition, the pore diameter of the micropores on the surface of the titanium material is smaller, the number of the micropores is reduced, and the structure is more compact after the titanium material is processed by the process.
The preparation method provided by the invention has the characteristics of simple process, low processing cost, high peanut forming speed, uniform size of the crystal flower, easiness in operation and the like, and can be applied to a large-scale industrial production line.
For further explanation of the present invention, the following detailed description of a pure titanium plate and a preparation method thereof is provided in connection with examples, but it should be understood that these examples are implemented on the premise of the technical proposal of the present invention, and detailed implementation and specific operation procedures are given only for further explanation of the features and advantages of the present invention, and not limitation of the claims of the present invention, and the scope of protection of the present invention is not limited to the following examples.
Example 1
A0.8 mm TA1 plate is adopted, and is subjected to blanking, stretching and trimming to prepare a cup body with the diameter of 80mm and the depth of 160mm, and a finished product is a titanium sheet product, and then the titanium sheet product is washed by Na (OH) alkali solution, washed by distilled water and dried by cold air. Placing the titanium cup into a vacuum furnace, and vacuumizing to 2.0X10 -3 Pa, heating to 600 ℃, and preserving heat for 1h; raising the temperature to 900 ℃ for the second time, and preserving the heat for 3 hours; then argon is injected for rapid cooling, the air pressure of the argon is 0.08MPa, and then the argon is cooled to 840 ℃ along with the furnace; finally, the scaly crystal flower with metallic luster is obtained, wherein the size of the crystal flower is 5.0-6.0 mm.
The titanium sheet prepared in example 1 of the present invention was characterized.
The result shows that the pore diameter of the micropores on the surface of the titanium material is smaller, the number of the micropores is reduced, and the structure is more compact after the titanium material is processed by the process. And the crystal structure of the titanium sheet after the treatment of the invention is still a low-temperature stable phase-alpha-Ti.
Example 2
A0.8 mm TA1 plate is adopted, and is subjected to blanking, stamping and trimming to prepare a rectangular disc-shaped finished product with the length of 300mm and the width of 160mm, wherein the finished product is a titanium sheet product, and then the titanium sheet product is washed by Na (OH) alkaline solution, washed by distilled water and dried by cold air. Placing the titanium cup into a vacuum furnace, and vacuumizing to 2.0X10 -3 Pa, heating to 600 ℃, and preserving heat for 1h; raising the temperature to 900 ℃ for the second time, and preserving the heat for 3 hours; then argon is injected for rapid cooling, the air pressure of the argon is 0.08MPa, and then the argon is cooled to 840 ℃ along with the furnace; finally, the scaly crystal flower with metallic luster is obtained, wherein the size of the crystal flower is 5.0-6.0 mm.
The foregoing has outlined rather broadly the principles and embodiments of the present invention in order that the detailed description of the invention may be better understood, and in order that the present invention may be practiced by anyone skilled in the art, including in any regard to the practice of the invention, including in any regard to the manufacture and use of such devices or systems, and in any regard to the practice of the invention. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims. The scope of the patent protection is defined by the claims and may include other embodiments that occur to those skilled in the art. Such other embodiments are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal language of the claims.
Claims (10)
1. The preparation method of the pure titanium plate is characterized by comprising the following steps of:
1) Under the vacuum condition, after the first temperature rise and heat preservation step and the second temperature rise and heat preservation step, the pure titanium sheet material is subjected to rapid air cooling quenching treatment, and then the pure titanium sheet material with the scaly crystal flower apparent structure on the surface is obtained;
the pure titanium plate is a pure titanium thin plate;
the thickness of the pure titanium plate is 0.4-2 mm;
the scaly crystal flowers are specifically scaly crystal flowers formed by martensitic transformation;
the surface metal crystal structure of the pure titanium sheet is low-temperature stable phase alpha-Ti;
the scaly crystal flower is cooled to the phase transition temperature T in the pure titanium plate by quenching β The following steps were carried out;
before quenching and cooling, the pure titanium plate is subjected to two-step heat treatment;
the shape and/or size of the scaly crystal flower is adjusted by controlling the technological parameters of heat treatment and the quenching speed;
the temperature rising rate of the first temperature rising and heat preserving is 5-30 ℃/s;
the temperature of the first heating and heat preservation is 550-650 ℃;
the heat preservation time of the first heating and heat preservation is 1-3 h;
the temperature rising rate of the second temperature rising and preserving is 5-30 ℃/s;
the heat preservation time of the second heating and heat preservation is more than 2.5 hours and less than or equal to 3.5 hours;
the heat preservation temperature of the second heating and heat preservation is T β ～950℃；
The rapid air cooling is specifically performed by adopting inert gas;
the cooling rate of the rapid air-cooling quenching treatment is 5-15 ℃/s;
the pure titanium plate is provided with a scaly crystal flower apparent structure on the surface;
the size of the scaly crystal flower is more than 3mm and less than or equal to 8mm.
2. The method according to claim 1, wherein,
the purity of the pure titanium plate is more than or equal to 99.6 percent of Ti.
3. The production method according to claim 1, wherein the flaky crystal flower is a flaky crystal flower having metallic luster;
the scaly crystal flowers are uniformly distributed scaly crystal flowers.
4. The method according to claim 1, wherein the roughness of the pure titanium plate surface is 0.3 to 0.6 μm.
5. The method of claim 1, wherein the pure titanium sheet material comprises pure titanium sheet or pure titanium sheet product.
6. The method according to claim 1, wherein the pure titanium thin plate raw material is a pretreated pure titanium thin plate raw material;
the pretreatment includes a buffing and/or decontamination step.
7. The method of claim 6, wherein the degree of sanding polishing is specular;
the roughness after the grinding and polishing is 0.3-0.6 mu m;
the decontamination mode comprises the steps of cleaning decontamination under ultrasonic waves by adopting alkali solution.
8. The method according to claim 1, wherein the vacuum pressure is 5.0X10 or less - 3 Pa；
The first heating and heat preserving step is a grain homogenization process.
9. The method of claim 1, wherein T is β Is 833-890 ℃;
the second heating and heat preserving step is a crystal grain regrowth process.
10. The method of claim 9, wherein the rapid air-cooled inert gas pressure is 0.05-0.15 MPa;
the cut-off temperature of the rapid air-cooled quenching is T β Temperature or lower.
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