CN114657365A - 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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- CN114657365A CN114657365A CN202210367037.2A CN202210367037A CN114657365A CN 114657365 A CN114657365 A CN 114657365A CN 202210367037 A CN202210367037 A CN 202210367037A CN 114657365 A CN114657365 A CN 114657365A
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- 239000010936 titanium Substances 0.000 title claims abstract description 138
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 130
- 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 89
- 238000003672 processing method Methods 0.000 title description 9
- 238000000034 method Methods 0.000 claims abstract description 30
- 230000008569 process Effects 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000004321 preservation Methods 0.000 claims description 35
- 238000001816 cooling Methods 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 31
- 238000010791 quenching Methods 0.000 claims description 16
- 230000000171 quenching effect Effects 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 238000005498 polishing Methods 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 10
- 230000007704 transition Effects 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 239000002932 luster Substances 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910000734 martensite Inorganic materials 0.000 claims description 4
- 238000005202 decontamination Methods 0.000 claims description 3
- 230000003588 decontaminative effect Effects 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 14
- 238000012545 processing Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 230000003373 anti-fouling effect Effects 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 12
- 229910052786 argon Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000001035 drying Methods 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
- 238000007664 blowing Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 238000004381 surface treatment 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 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
- 239000007858 starting material Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000009966 trimming 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
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 scale-shaped crystal flower has a size of more than 3mm and less than or equal to 8 mm. The pure titanium sheet has scale-shaped crystal flowers with specific sizes, and the crystal flowers are uniform in size and standard in shape. And the surface of the crystal flower has the characteristics of high smoothness, strong anti-fouling capability, no surface blackening for a long time and strong oxidation resistance. After the processing of the process, the metal crystal structure on the surface of the titanium sheet is not changed and is alpha-Ti which is a low-temperature stable phase. In addition, the titanium material processed by the process has small surface micropore diameter, reduced number and more compact structure. The preparation method provided by the invention has the characteristics of simple process, low processing cost, high crystal flower generation speed, uniform crystal flower size, 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 surface heat treatment of pure titanium sheets, 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 demand of consumers on the titanium product, the surface of the titanium product also needs to be diversified urgently. In addition, the titanium product with the natural color of metal has the defect of blackening along with surface oxidation. The crystal flower treatment on the surface of the titanium sheet can not only make the titanium product more beautiful, but also overcome the defect that the surface of the titanium product is blackened.
Some improved schemes are also disclosed in the prior technical scheme, such as a preparation method of a titanium product needle-shaped crystal pattern, but the preparation method is complex, a heating and heat-preserving process needs to be carried out in three stages, the treatment process efficiency is low, the three processing times consume as much as 16 hours and at least 3.75 hours, the energy consumption is high, and the preparation method is not environment-friendly. The technical scheme also discloses a processing method of titanium product crystal patterns, but in the preparation process, the temperature is directly increased to over 1000 ℃, so that the crystal growth speed is too high, and the grain size distribution and the shape uniformity of crystal grains cannot 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. In addition, after the heat treatment, the process needs to add high-pollution procedures such as polishing, acid pickling and etching to obtain the 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 the phenomenon of non-uniformity also exists in acid cleaning and etching.
Therefore, how to find a more suitable preparation process for the pure titanium plate surface crystal flower to solve the above technical problems, especially, how to be suitable for a pure titanium sheet, has become one of the problems to be solved urgently 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 plate and a preparation method thereof, especially a pure titanium thin plate with surface crystal patterns. The pure titanium sheet provided by the invention has the characteristics of scale-shaped crystal flowers with specific sizes, uniform crystal flower size, high surface smoothness of the crystal flowers, strong anti-fouling capability, no blackening of the surface for a long time and strong oxidation resistance. Meanwhile, the preparation process is simple, the processing cost is low, the crystal flower generation 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 scale-shaped crystal flower has a size of more than 3mm and less than or equal to 8 mm.
Preferably, the pure titanium plate is a pure titanium sheet;
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 scale-shaped crystal flowers are specifically scale-shaped crystal flowers formed by martensite transformation;
the scale-shaped crystal flower is a scale-shaped crystal flower with metallic luster;
the scale-shaped crystal flowers are uniformly distributed.
Preferably, the scaly crystal flowers are quenched and cooled to the phase transition temperature T on the pure titanium plateβObtained by the following steps;
before quenching and cooling, the pure titanium plate only needs two-step heat treatment;
the shape and/or size of the scale-shaped crystal flower is adjusted by controlling the technological parameters of heat treatment and the quenching rate;
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, carrying out a first heating and heat preservation step and a second heating and heat preservation step on a pure titanium sheet raw material, and then carrying out rapid air cooling quenching treatment to obtain a pure titanium sheet with a scaly crystal flower apparent structure on the surface;
and the heat preservation time of the second temperature rise and heat preservation is more than 2.5 hours and less than or equal to 3.5 hours.
Preferably, the pure titanium sheet raw material comprises a pure titanium sheet or a pure titanium sheet product;
the pure titanium sheet raw material is a pretreated pure titanium sheet raw material;
the pre-treatment comprises a polishing and/or desmearing step.
Preferably, the grinding and polishing degree is a mirror surface;
the roughness after grinding and polishing is 0.3-0.6 mu m;
the decontamination mode comprises the step of cleaning and decontaminating by adopting an alkali solution under ultrasonic waves.
Preferably, the pressure of the vacuum is 5.0X 10 or less-3Pa；
The temperature rise rate of the first temperature rise and preservation is 5-30 ℃/s;
the heat preservation temperature of the first temperature rise and heat preservation is 550-650 ℃;
the heat preservation time of the first temperature rise and heat preservation is 1-3 h;
the first temperature raising and preserving step is a crystal grain homogenizing process.
Preferably, the temperature rise rate of the second temperature rise and preservation is 5-30 ℃/s;
the heat preservation temperature of the second temperature rise and heat preservation is Tβ～950℃；
The T isβ833 to 890 ℃;
the second temperature raising and maintaining step is a crystal grain regrowth process.
Preferably, the rapid air cooling is rapid air cooling by using inert gas;
the pressure of the rapidly air-cooled inert gas 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-cooling quenching is TβBelow the temperature.
The invention provides a pure titanium plate, which is a pure titanium plate with a scaly crystal flower apparent structure on the surface; the scale-shaped crystal flower has a size of more than 3mm and less than or equal to 8 mm. Compared with the prior art, the pure titanium sheet provided by the invention has scale-shaped crystal flowers with specific sizes, the crystal flowers are uniform in size and standard in shape. And the surface of the crystal flower has the characteristics of high smoothness, strong anti-fouling capability, no surface blackening for a long time and strong oxidation resistance.
The invention also provides a processing method of the pure titanium sheet surface crystal flower, the titanium sheet obtains a uniform surface treatment process of the sheet crystal flower on the surface of the titanium sheet product by controlling the heating process twice and the heat preservation time under the vacuum environment and controlling the cooling speed of the titanium sheet, and the obtained crystal flower has the characteristics of high surface smoothness, uniform crystal flower size, strong anti-pollution capability, no surface blackening for a long time and strong oxidation resistance. After the processing of the process, the metal crystal structure on the surface of the titanium sheet is not changed and is alpha-Ti which is a low-temperature stable phase. In addition, the pore diameter of micropores on the surface of the titanium material is reduced, the number of the micropores is reduced, and the structure is more compact.
The preparation method provided by the invention has the characteristics of simple process, low processing cost, high crystal flower generation speed, uniform crystal flower size, 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 invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
All raw materials of the invention are not particularly limited in purity, and the invention preferably adopts the purity requirement which is conventional in the field of preparing industrial pure or pure titanium plates.
All the raw materials, the marks and the acronyms thereof belong to the conventional marks and acronyms in the field, each mark and acronym is clear and definite in the field of related application, and the raw materials can be purchased from the market or prepared by a conventional method by the technical staff in the field according to the marks, the acronyms and the corresponding application.
The process used in the invention belongs to the field of general abbreviation, the specific steps and general parameters of each abbreviation are clear and definite in the related field, and the technicians in the field can realize the process by the general method according to the abbreviation.
The invention provides a pure titanium plate which has a scaly crystal flower apparent structure on the surface.
The scale-shaped crystal flower has a size of more than 3mm and less than or equal to 8 mm.
In the invention, the scale-like crystal flower preferably has a size of 3-8 mm, more preferably 4-7 mm, and even more preferably 5-6 mm.
In the present invention, the pure titanium plate is preferably a pure titanium thin plate.
In the invention, the thickness of the pure titanium plate is preferably 0.4-2 mm, more preferably 0.7-1.7 mm, and more preferably 1.0-1.4 mm.
In the present invention, the purity of the pure titanium plate is preferably 99.6% or more of Ti, more preferably 99.7% or more of Ti, and still more preferably 99.8% or more of Ti.
In the present invention, the scale-like florets are preferably scale-like florets formed by martensitic transformation.
In the present invention, the scale-like florets are preferably scale-like florets having a metallic luster.
In the present invention, the scale-like florets are preferably uniformly distributed scale-like florets.
In the invention, the scaly crystal flowers are preferably quenched and cooled to the phase transition temperature T on a pure titanium plateβObtained as follows. Wherein, the phase transition temperature T in the inventionβWhich is the concept of phase transition temperature of pure titanium well known to those skilled in the art. In particular, TβThe transition 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 present invention, the pure titanium plate preferably only needs to be subjected to two heat treatments before the quenching and cooling.
In the present invention, the shape and/or size of the scale-like florets are preferably adjusted by controlling the process parameters of the heat treatment and the quenching rate.
In the invention, the roughness of the surface of the pure titanium plate is preferably 0.3-0.6 μm, more preferably 0.35-0.55 μm, and more preferably 0.4-0.5 μm.
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 raw 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 to obtain the pure titanium sheet with the scaly crystal flower apparent structure on the surface.
In the present invention, the holding time of the second temperature raising and holding is greater than 2.5 hours and not more than 3.5 hours, more preferably greater than 2.7 hours and not more than 3.3 hours, and still more preferably greater 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 polish and/or stain removal step, more preferably a polish and stain removal step.
In the present invention, the degree of the grinding and polishing is preferably a mirror surface.
In the invention, the roughness after grinding and polishing is preferably 0.3-0.6 μm, more preferably 0.35-0.55 μm, and more preferably 0.4-0.5 μm.
In the present invention, the decontamination means preferably includes cleaning with an alkali solution under ultrasonic waves.
In the present invention, the pressure of the vacuum is preferably 5.0X 10 or less-3Pa。
In the invention, the temperature rise rate of the first temperature rise and heat preservation is preferably 5-30 ℃/s, more preferably 10-25 ℃/s, and more preferably 15-20 ℃/s.
In the invention, the heat preservation temperature of the first temperature rise and heat preservation is preferably 550-650 ℃, more preferably 570-630 ℃, and more preferably 590-610 ℃.
In the invention, the first temperature rise and heat preservation time is preferably 1-3 h, more preferably 1.4-2.6 h, and more preferably 1.8-2.2 h.
In the present invention, the first temperature raising and holding step is preferably a crystal grain homogenization process.
In the invention, the temperature rise rate of the second temperature rise and preservation is preferably 5-30 ℃/s, more preferably 10-25 ℃/s, and more preferably 15-20 ℃/s.
In the present invention, the holding temperature of the second temperature raising and holding is preferably TβAbout 950 ℃, more preferably Tβ930 ℃ and more preferably Tβ～910℃。
In the present invention, said TβPreferably 833-890 ℃, more preferably 843-880 ℃, and more preferably 853-870 ℃.
In the invention, the second temperature raising and maintaining step is preferably a crystal grain regrowth process.
In the present invention, the rapid air cooling is preferably performed by using an inert gas.
In the invention, the pressure of the rapidly air-cooled inert gas is preferably 0.05-0.15 MPa, more preferably 0.07-0.13 MPa, and more preferably 0.09-0.11 MPa.
In the invention, the cooling rate of the rapid air-cooling quenching treatment is preferably 5-15 ℃/s, more preferably 7-13 ℃/s, and more preferably 9-11 ℃/s.
In the present invention, the cut-off temperature of the rapid air-cooling quenching is preferably TβBelow the temperature.
In the present invention, said TβPreferably 833-890 ℃, more preferably 843-880 ℃, and more preferably 853-870 ℃.
The invention provides a better complete and refined integral processing method, which ensures the uniformity and the size uniformity of flaky crystal flowers on the surface of a pure titanium sheet and better improves the apparent characteristics and the sheet performance of the pure titanium sheet, and the preparation method of the pure titanium sheet can specifically comprise the following steps:
the invention provides a processing method of pure titanium sheet (Ti is more than or equal to 99.6 percent and the thickness is 0.4 mm-2 mm) surface crystal flower, which comprises the following steps:
a. grinding and polishing: grinding and polishing the surface of a titanium sheet or a titanium plate product, wherein the polishing degree is a mirror surface, and the roughness is 0.3-0.6 mu m;
b. degreasing: cleaning the residual oil stain on the surface by using an alkali solution, and drying by cold air for later use after cleaning;
c. and (3) heat treatment environment: placing the cleaned and dried titanium sheet or titanium sheet product in a vacuum heating furnace, wherein the air pressure in the furnace is 5.0 multiplied by 10-3Pa or less.
d. Grain homogenization: heating for the first time, heating the titanium sheet or the titanium plate product to 550-650 ℃ in a vacuum heating furnace, and preserving heat for 2 hours;
e. and (3) growing crystal grains again: continuously heating to TβThe temperature is kept at 950 ℃ for more than 2.5 hours and less than or equal to 3.5 hours;
f. quenching treatment: after heat preservation, argon is introduced to reduce the temperature to the phase transition temperature TβAnd continuously air-cooling to 80-100 ℃, and taking out.
Specifically, the cleaning in step b is performed by first cleaning with an alkali solution under ultrasonic waves, and then rinsing with flowing distilled water.
In particular, the vacuum furnace in step cThe internal air pressure may be 5.0 × 10-3Pa, more preferably 2.0X 10-3The vacuum effect of Pa is better.
Specifically, the temperature rise speed of the vacuum furnace in the step d is 5-30 ℃/s, the volume size of the titanium metal crystal can be homogenized in the process, and a tissue with the same size is obtained to prepare for the next reaction.
In particular, T in step eβThe transition temperature of alpha-beta phase of pure titanium metal is 833-890 ℃, the transition temperature of alpha-beta phase of pure titanium is dependent on the influence factors of heating temperature, heating speed, cooling speed, different batches and the like, the surface microscopic atomic rearrangement phenomenon occurs in the secondary growth process of pure titanium metal crystal, and the surface fine defects are eliminated along with the growth of the crystal size and volume.
Specifically, the pressure of the argon introduced in the step f is 0.05-0.15 MPa, the cooling speed is gentle, the titanium metal is subjected to martensite phase transformation through a phase transformation interval, 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, the scale-shaped crystal flowers are uniform in size, and the scale-shaped crystal flowers are stored; different air pressures can make the titanium metal obtain different cooling rates, so that the secondary heat preservation temperature can be adjusted accordingly.
The pure titanium sheet with the surface crystal flowers and the processing method thereof are provided by the steps of the invention, and the pure titanium sheet prepared by the invention has the scale-shaped crystal flowers with specific sizes, the crystal flowers are uniform in size and standard in shape. And the surface of the crystal flower has the characteristics of high smoothness, strong anti-fouling capability, no surface blackening for a long time and strong oxidation resistance.
According to the processing method of the pure titanium sheet surface crystal flower, the titanium sheet is subjected to a uniform surface treatment process of the sheet crystal flower on the surface of a titanium sheet product by controlling the heating process twice and the heat preservation time and controlling the cooling speed of the titanium sheet in a vacuum environment, and the obtained crystal flower has the characteristics of high surface smoothness, uniform crystal flower size, strong anti-pollution capability, no surface blackening for a long time and strong oxidation resistance. After the processing of the process, the metal crystal structure on the surface of the titanium sheet is not changed and is alpha-Ti which is a low-temperature stable phase. In addition, the pore diameter of micropores on the surface of the titanium material is reduced, the number of the micropores is reduced, and the structure is more compact.
The preparation method provided by the invention has the characteristics of simple process, low processing cost, high crystal flower generation speed, uniform crystal flower size, easiness in operation and the like, and can be applied to a large-scale industrial production line.
For further illustration of the present invention, the following will describe a pure titanium plate and its preparation method in detail with reference to the following examples, but it should be understood that these examples are implemented on the premise of the technical solution of the present invention, and the detailed embodiments and specific operation procedures are given, which are only for further illustration of the features and advantages of the present invention, but not for 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 made into a cup body with the diameter of 80mm and the depth of 160mm through blanking, stretching and trimming, the finished product is a titanium sheet product, and then the titanium sheet product is cleaned by Na (OH) alkali solution, distilled water and cold air for drying. Putting the titanium cup into a vacuum furnace, and vacuumizing to 2.0 multiplied by 10-3Pa, heating to 600 ℃, and keeping the temperature for 1 h; heating to 900 ℃ for the second time, and keeping the temperature for 3 hours; then, filling argon gas for rapid cooling, wherein the blowing pressure of the argon gas is 0.08MPa, and then cooling to 840 ℃ along with the furnace; finally obtaining the scaly crystal flower with metallic luster, wherein the size of the crystal flower is 5.0-6.0 mm.
The titanium sheet prepared in example 1 of the invention was characterized.
The result shows that the titanium material processed by the process has small surface micropore diameter, reduced number of micropores and more compact tissue. And the crystal structure of the titanium material 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, blanking, stamping and edge cutting are carried out, a rectangular disc-shaped finished product with the length of 300mm and the width of 160mm is prepared, the finished product is a titanium sheet product, and then the titanium sheet product is cleaned by Na (OH) alkali solution, distilled water and cold air for drying. Putting the titanium cup into a vacuum furnace, and vacuumizing to 2.0 multiplied by 10-3Pa, heating to 600 ℃, and keeping the temperature for 1 h;heating to 900 ℃ for the second time, and keeping the temperature for 3 hours; then, filling argon gas for rapid cooling, wherein the blowing pressure of the argon gas is 0.08MPa, and then cooling to 840 ℃ along with the furnace; finally obtaining the scaly crystal flower with metallic luster, wherein the size of the crystal flower is 5.0-6.0 mm.
While the present invention has been described in detail with respect to a pure titanium sheet with surface texturing and a method of making the same, the present invention is described in detail with reference to specific examples, which are included to facilitate the understanding of the principles of the present invention and its core concepts, including the best mode, and to enable any person skilled in the art to practice the invention, including making and using any devices or systems and performing any incorporated methods. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention. The patentable scope of the invention is defined by the claims, and may include other examples 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 languages of the claims.
Claims (10)
1. The pure titanium plate is characterized in that the pure titanium plate is a pure titanium plate with a scaly crystal flower apparent structure on the surface;
the scale-shaped crystal flower has a size of more than 3mm and less than or equal to 8 mm.
2. The pure titanium plate of claim 1, wherein said pure titanium plate is a pure titanium sheet;
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.
3. The pure titanium plate according to claim 1, wherein the scale-like flower is specifically a martensite transformation-formed scale-like flower;
the scale-shaped crystal flower is a scale-shaped crystal flower with metallic luster;
the scale-shaped crystal flowers are uniformly distributed.
4. The pure titanium plate of claim 1, wherein the scale-like crystal grains are quenched and cooled to a phase transition temperature T in the pure titanium plateβObtained by the following steps;
before quenching and cooling, the pure titanium plate only needs two-step heat treatment;
the shape and/or size of the scale-shaped crystal flower is adjusted by controlling the technological parameters of heat treatment and the quenching rate;
the roughness of the surface of the pure titanium plate is 0.3-0.6 mu m.
5. The preparation method of the pure titanium plate is characterized by comprising the following steps:
1) under the vacuum condition, carrying out a first heating and heat preservation step and a second heating and heat preservation step on a pure titanium sheet raw material, and then carrying out rapid air cooling quenching treatment to obtain a pure titanium sheet with a scaly crystal flower apparent structure on the surface;
and the heat preservation time of the second temperature rise and heat preservation is more than 2.5 hours and less than or equal to 3.5 hours.
6. The method according to claim 5, wherein the pure titanium sheet raw material comprises a pure titanium sheet or a pure titanium sheet product;
the pure titanium sheet raw material is a pretreated pure titanium sheet raw material;
the pre-treatment comprises a polishing and/or desmearing step.
7. The production method according to claim 6, wherein the degree of the grinding and polishing is a mirror surface;
the roughness after grinding and polishing is 0.3-0.6 mu m;
the decontamination mode comprises the step of cleaning and decontaminating by adopting an alkali solution under ultrasonic waves.
8. The method of claim 5, wherein the vacuum has a pressure of 5.0 x 10 or less- 3Pa；
The temperature rise rate of the first temperature rise and preservation is 5-30 ℃/s;
the heat preservation temperature of the first temperature rise and heat preservation is 550-650 ℃;
the heat preservation time of the first temperature rise and heat preservation is 1-3 h;
the first temperature raising and preserving step is a crystal grain homogenizing process.
9. The preparation method according to claim 5, wherein the temperature rise rate of the second temperature rise and preservation is 5-30 ℃/s;
the heat preservation temperature of the second temperature rise and heat preservation is Tβ～950℃；
The T isβ833 to 890 ℃;
the second temperature raising and maintaining step is a crystal grain regrowth process.
10. The preparation method according to claim 9, wherein the rapid air cooling is specifically rapid air cooling using an inert gas;
the pressure of the rapidly air-cooled inert gas 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-cooling quenching is TβBelow the temperature.
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