CN113458144A - Preparation method of titanium belt for bulging of vacuum cup - Google Patents
Preparation method of titanium belt for bulging of vacuum cup Download PDFInfo
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- CN113458144A CN113458144A CN202110746986.7A CN202110746986A CN113458144A CN 113458144 A CN113458144 A CN 113458144A CN 202110746986 A CN202110746986 A CN 202110746986A CN 113458144 A CN113458144 A CN 113458144A
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- 238000005242 forging Methods 0.000 claims abstract description 24
- 238000005097 cold rolling Methods 0.000 claims abstract description 23
- 238000005238 degreasing Methods 0.000 claims abstract description 23
- 238000005266 casting Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000005554 pickling Methods 0.000 claims abstract description 14
- 238000005098 hot rolling Methods 0.000 claims abstract description 12
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- 238000000034 method Methods 0.000 claims description 58
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B15/00—Arrangements for performing additional metal-working operations specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/02—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
-
- 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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
- C23G1/205—Other heavy metals refractory metals
Abstract
The invention discloses a preparation method of a titanium belt for bulging of a vacuum cup, and belongs to the technical field of titanium metal vacuum cups. The preparation method of the titanium strip for the bulging of the vacuum cup comprises the following steps: performing EB (electron beam) casting on a titanium sponge raw material, and forging a formed cast ingot to obtain a titanium slab; carrying out hot rolling on the titanium plate blank to obtain a hot-rolled titanium coil, and carrying out annealing and acid pickling on the hot-rolled titanium coil; carrying out cold rolling on the acid-washed hot-rolled titanium coil, and carrying out chemical and ultrasonic combined degreasing treatment after the cold rolling to obtain a rolled hard titanium strip; annealing the rolled hard titanium belt to obtain an annealed titanium belt; and straightening the annealed titanium belt to prepare a plate with the wave height of less than or equal to 8mm and the arch of less than or equal to 10mm, thus obtaining the titanium belt for the bulging of the vacuum cup. The titanium belt for the bulging of the vacuum cup, prepared by the invention, has the characteristics of good plasticity, high grain size, uniform rolling performance and good bulging performance, the bulging qualification rate can reach 97%, and the problem of orange peel does not occur on the bulging surface.
Description
Technical Field
The embodiment of the application relates to the technical field of titanium metal vacuum cup preparation, in particular to a preparation method of a titanium belt for vacuum cup bulging.
Background
With the continuous improvement of the living standard of people, people pay more attention to health and life quality. The materials of the vacuum cup are widely researched, and the titanium metal material has the advantages of safety, no toxicity, high strength, corrosion resistance, non-dissolution, excellent antibacterial performance, good biocompatibility and the like, so that the titanium metal material can be used for replacing the traditional stainless steel material to prepare the vacuum cup. The titanium metal vacuum cup can not react with drinks such as tea leaves and carbonated beverages in the cup, can not dissolve out any heavy metal elements, and can not generate peculiar smell, so that the titanium metal vacuum cup can be used for making tea, making coffee, making milk and the like, can also be used for containing fruit juice, soybean milk, carbonated beverages, stew, traditional Chinese medicines and the like, and the titanium metal vacuum cup has become a trend to replace a stainless steel vacuum cup.
At present, the vacuum cups are generally prepared by adopting titanium seamless tubes and adopting a bulging process, but the titanium seamless tubes are expensive and are not beneficial to large-scale application and popularization, and the bulging qualification rate of the titanium seamless tubes can only reach 70-80 percent generally and cannot meet the bulging requirement for preparing the vacuum cups, so that the trend of preparing the vacuum cups by adopting titanium welded tubes instead of the titanium seamless tubes is already.
However, because the titanium metal material has poor processing plasticity and extensibility, the vacuum cup is easy to crack in a bulging weld joint area in the process of preparing the vacuum cup by using the titanium welded pipe, multiple bulging is needed, the bulging qualification rate is extremely low, and the problem that orange peel is easy to appear on the bulging surface of the titanium welded pipe is solved.
Disclosure of Invention
The purpose of the embodiment of the application is as follows: the preparation method of the titanium strip for the bulging of the vacuum cup is provided, and is used for solving the technical problems that a bulging weld joint area is easy to crack and an orange peel is easy to appear on a bulging surface when the vacuum cup is prepared by using the conventional titanium welded pipe.
In order to achieve the above purpose, the technical solution of the embodiment of the present application is:
the preparation method of the titanium strip for the bulging of the vacuum cup provided by the embodiment of the application comprises the following steps:
preparing a plate blank: performing EB (electron beam) casting on a titanium sponge raw material, and forging a formed cast ingot to obtain a titanium slab;
preparing a titanium coil: carrying out hot rolling on the titanium plate blank to obtain a hot-rolled titanium coil, and carrying out annealing and acid pickling on the hot-rolled titanium coil;
cold rolling and forming: carrying out cold rolling on the pickled hot-rolled titanium coil, and carrying out chemical and ultrasonic combined degreasing treatment after the cold rolling to obtain a rolled hard titanium strip;
annealing of a finished product: annealing the rolled hard titanium belt to obtain an annealed titanium belt;
straightening the titanium belt: and straightening the annealed titanium belt to prepare a plate with the wave height of less than or equal to 8mm and the arch of less than or equal to 10mm, thus obtaining the titanium belt for the bulging of the vacuum cup.
As a further improvement of the embodiment of the present application, the cold rolling forming includes a first rolling pass rolling and a second rolling pass rolling;
the first rolling pass rolling comprises: at 200-2Under the tension of the steel strip, carrying out 5-7 times of rolling on the pickled hot-rolled titanium coil, and carrying out annealing pickling after rolling to obtain a first rolling process rolled titanium strip;
the second rolling pass comprises: at 160-2Under the tension of (2), rolling the titanium strip rolled in the first rolling process for 8 to 15 times, and rollingAnd then carrying out chemical and ultrasonic combined degreasing treatment to obtain the rolled hard titanium belt.
As a further improvement of the embodiment of the present application, the chemical and ultrasonic combined degreasing treatment includes:
carrying out alkali liquor soaking treatment on the titanium belt obtained by 8-15 passes of rolling, and then carrying out alkali liquor cleaning under the ultrasonic condition;
carrying out alkali liquor washing treatment on the titanium belt washed by the alkali liquor, and carrying out ultrasonic water washing after the alkali liquor washing treatment;
and rinsing the titanium strip subjected to ultrasonic water washing with hot water, and drying the titanium strip with hot air after rinsing with hot water to obtain the rolled hard titanium strip.
As a further improvement of the embodiment of the application, the pass deformation of the first rolling process is 7-20%, and the total deformation of the hot-rolled titanium coil in the first rolling process is more than or equal to 40%.
As a further improvement of the embodiment of the application, the annealing mode in the first rolling process rolling procedure is continuous annealing, the temperature of the continuous annealing is 680-750 ℃, and the speed is 6-15 m/min.
As a further improvement of the embodiment of the application, the pass deformation of the second rolling process is 5-17%, and the total deformation of the titanium strip rolled by the first rolling process in the second rolling process is more than or equal to 50%.
As a further improvement of the embodiment of the present application, an annealing manner in the finished product annealing process is a hood-type annealing under inert gas protection, and the hood-type annealing includes:
under the protection of inert gas, annealing the hard titanium rolling strip at the temperature of 400-500 ℃ for 4-6h, and then heating to the temperature of 600-650 ℃ for annealing for 8-15 h.
As a further improvement of the embodiment of the application, the granularity of the titanium sponge raw material is 3-12.7mm, and HBW10/1500/30 is not more than 95.
As a further improvement of the embodiments of the present application, the preparation of the slab comprises:
performing EB fusion casting on the titanium sponge raw material to obtain 500mm & ltx & gt 1400 & lt- & gt 1450mm & ltx & gt L ingot casting, forging the ingot casting by using a forging press to obtain 180 mm & ltx & gt 950 & lt- & gt 1250mm & ltx & gt L titanium plate blanks, and finally performing machining on the titanium plate blanks to obtain the titanium plate blanks with the processing amount of the single surfaces of the two side surfaces being more than or equal to 5mm, the processing amount of the single surfaces of the two large surfaces being more than or equal to 7mm, the integral surface roughness being less than or equal to 6.3 mu m, and the whole surfaces being visible and having no oxide skin.
As a further improvement of the embodiment of the present application, the prepared titanium slab comprises the following chemical components:
ti is more than or equal to 99.6 wt%; and impurities
Fe is less than or equal to 0.05 wt%, C is less than or equal to 0.03 wt%, N is less than or equal to 0.01 wt%, H is less than or equal to 0.006 wt%, O is less than or equal to 0.06 wt%, others are less than or equal to 0.1 wt%, and the total amount of impurities is less than or equal to 0.4 wt%.
Compared with the prior art, the advantages or beneficial effects of the embodiments of the present application at least include:
according to the preparation method of the titanium belt for the bulging of the vacuum cup, the titanium plate blank is prepared from the titanium sponge raw material in the mode of combining EB (electron beam) casting and forging, and then hot rolling, annealing and acid pickling, cold rolling forming and degreasing, finished product annealing and straightening treatment are sequentially carried out on the titanium plate blank, so that the titanium belt for the bulging of the vacuum cup is prepared, the processing plasticity and the extensibility of the titanium belt are modified, the operation is simple, the cost is low, and the preparation method is suitable for industrial production.
The titanium belt for the bulging of the vacuum cup prepared by the invention has the characteristics of good plasticity, high grain size, uniform whole-rolling performance and good bulging performance. Research shows that the bulging qualification rate of the titanium belt for the bulging of the vacuum cup can reach more than 97 percent, multiple bulging treatment is not needed, the problem of orange peel does not occur on the bulging surface, the transverse yield strength is less than or equal to 250Mpa, and the transverse elongation (A) is50) More than or equal to 35 percent, and the grain size can reach 6 grades and above.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings used in the description of the embodiments will be briefly introduced below. It is obvious that the drawings in the following description are only some of the embodiments described in the present application, and that other drawings can be derived from these drawings by a person skilled in the art without inventive effort.
FIG. 1 is a process flow chart for preparing a titanium strip for vacuum cup bulging according to an embodiment of the present application;
FIG. 2 is a microscopic structure view of a titanium band for bulging in a vacuum cup manufactured in example 1 of the present application;
FIG. 3 is a microscopic structure view of a titanium ribbon for cup bulging prepared in example 2 of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. It should be apparent that the embodiments described below are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be appreciated by those skilled in the art that the titanium sponge starting material described in the examples below is titanium sponge obtained from commercial sources or prepared by routine experimentation.
As shown in fig. 1, the method for preparing a titanium band for vacuum cup bulging provided in this embodiment specifically includes steps S101 to S105.
S101, preparing a plate blank: and after EB (electron beam) casting is carried out on the sponge titanium raw material, forging the formed cast ingot to obtain a titanium slab. Preferably, in this embodiment, the titanium sponge raw material is cast in an EB furnace (electron beam cold bed furnace) to obtain an ingot of 500mm × 1400-; and (3) carrying out machining treatment on the titanium plate blank to obtain the titanium plate blank with the single-side machining amount of two side surfaces being more than or equal to 5mm, the single-side machining amount of two large surfaces being more than or equal to 7mm, the integral surface roughness being less than or equal to 6.3 mu m, and the whole surface being exposed to light and not leaving oxide skin. Wherein the titanium sponge raw material is 0A grade, the granularity of the titanium sponge raw material is 3-12.7mm, and the HBW10/1500/30 is not more than 95.
The nature, amount, existence state, distribution and shape of impurities contained in titanium metal affect the working plasticity of titanium metal. Therefore, in this embodiment, the raw materials are selected and the titanium slab is prepared by combining EB fusion casting and forging, so that the chemical composition of the prepared titanium slab is as follows:
ti is more than or equal to 99.6 wt%; and impurities
Fe is less than or equal to 0.05 wt%, C is less than or equal to 0.03 wt%, N is less than or equal to 0.01 wt%, H is less than or equal to 0.006 wt%, O is less than or equal to 0.06 wt%, others are less than or equal to 0.1 wt%, and the total amount of impurities is less than or equal to 0.4 wt%.
It will be understood by those skilled in the art that the processing plasticity of titanium metal increases with increasing purity, and that the nature, quantity, presence, and distribution and shape of impurities contained in titanium metal all contribute to the processing plasticity of titanium metal. Therefore, in the embodiment, the titanium slab is prepared by combining the EB furnace casting and the forging, and the high-density and low-density impurities contained in the titanium sponge can be sufficiently removed by the EB furnace casting, so that the titanium purity of the prepared titanium slab is improved; and forging can change the molten state structure and the size and uniformity of crystal grains, and further enhance the processing plasticity and impact strength of the titanium slab, so that the titanium slab with excellent comprehensive properties such as processing plasticity, impact strength and the like is prepared. That is to say, in this embodiment, the titanium slab is prepared by combining EB casting and forging, which not only takes the advantages of controlling high-density and low-density impurities contained in the sponge titanium raw material by EB furnace casting into account, but also improves the casting state structure by forging, thereby realizing the processing plasticity and grain structure modification of the titanium slab. The EB furnace smelting is a smelting method for bombarding molten metal by taking an accelerated electron beam as a heat source so as to convert the kinetic energy of electrons into heat energy to heat and melt the metal.
S102-preparing a titanium roll: and carrying out hot rolling on the titanium plate blank to obtain a hot-rolled titanium coil, and carrying out annealing and acid pickling on the hot-rolled titanium coil. Preferably, in the present embodiment, the titanium slab is hot-rolled using a steckel mill to obtain a hot-rolled titanium coil having a thickness of 4.0mm, and then the hot-rolled titanium coil is subjected to continuous annealing pickling to obtain a pickled hot-rolled titanium coil of 4.0 × 1250 × C. Wherein the hot rolling temperature is 860 ℃, and the annealing process is 750 ℃ multiplied by 15 m/min.
S103-cold rolling and forming: to acid pickling stationAnd cold rolling the hot-rolled titanium coil, and performing chemical and ultrasonic combined degreasing treatment after the cold rolling to obtain the rolled hard titanium strip. Preferably, the present embodiment performs two-pass rolling (i.e., a first pass and a second pass) on the pickled hot-rolled titanium coil by using twenty-high rolling. Wherein the first rolling pass rolling comprises: the rolling force is 3000-4500kN, the tension is 200-240N/mm2And under the condition that the speed is 80-220m/min, carrying out 5-7 times of rolling on the pickled hot-rolled titanium coil, and carrying out annealing pickling (the annealing process is 750 ℃ multiplied by 15m/min) after rolling to obtain the first rolling process rolled titanium belt. The second rolling pass comprises: the rolling force is 3000-4500kN, and the tension is 160-190N/mm2And under the condition that the speed is 80-220m/min, carrying out 8-15 times of rolling on the titanium strip rolled by the first rolling process, and carrying out chemical and ultrasonic combined degreasing treatment after rolling to obtain the rolled hard titanium strip.
In the cold-rolling deformation of a metal, the working plasticity of the metal decreases as the degree of deformation increases. In view of the above, the inventor of the present invention studied the influence of the rolling deformation on the bulging qualification rate of the produced titanium strip for the bulging of the vacuum cup in the two-rolling process, and the results show that: when the pass deformation of the first rolling process rolling is 7-20%, and the total deformation of the hot-rolled titanium coil in the first rolling process is more than or equal to 40%, the bulging qualification rate of the produced titanium belt for the bulging of the vacuum cup is improved in the same ratio; when the pass deformation of the second rolling process is 5-17%, and the total deformation of the titanium strip rolled by the first rolling process in the second rolling process is more than or equal to 50%, the bulging qualification rate of the produced titanium strip for bulging the vacuum cup is obviously improved in the same ratio. Therefore, in the embodiment, the pass deformation of the first rolling pass is preferably controlled to be 7-20%, the total deformation of the hot-rolled titanium coil in the first rolling pass is preferably controlled to be more than or equal to 40%, the pass deformation of the second rolling pass is preferably controlled to be 5-17%, and the total deformation of the first rolling pass rolled titanium strip in the second rolling pass is preferably controlled to be more than or equal to 50%.
It should be noted that, in the present embodiment, rolling oil is removed by a degreasing method combining chemistry and ultrasonic waves, and preferably, the degreasing device for removing rolling oil is composed of a soaking tank, a first cleaning tank, a brushing tank, a second cleaning tank and a rinsing tank, and cleaning liquid components related to the degreasing device are shown in table 1.
TABLE 1 cleaning solution composition for degreasing equipment
| Process tank | Cleaning liquid | KOH concentration | Temperature of | Time | Whether or not to ultrasonically treat |
| Soaking tank | KOH + additive | 1.8±0.2％ | 60±5℃ | - | |
| First cleaning tank | KOH + additive | 1.8±0.2％ | 60±5℃ | Ultrasonic wave | |
| Brushing groove | KOH + additive | 1.8±0.2％ | 60±5℃ | - | |
| The second cleaning tank | Water (W) | - | 60±5℃ | Ultrasonic wave | |
| Rinsing tank | Water (W) | - | 60±5℃ | - |
As can be seen from table 1 above, the degreasing process by combining chemical treatment and ultrasonic treatment in this embodiment includes steps S1031 to S1033.
S1031: carrying out alkali liquor soaking treatment on the titanium belt which is rolled for 8-15 times in the soaking tank, then transferring the titanium belt into the first cleaning tank, and carrying out alkali liquor cleaning under the ultrasonic condition;
s1032: carrying out alkali liquor washing treatment on the titanium belt washed by the alkali liquor in the washing tank, and after the alkali liquor washing treatment, transferring the titanium belt into the second washing tank for ultrasonic washing;
s1033: and rinsing the ultrasonically washed titanium strip with hot water in the rinsing tank, and drying the titanium strip with hot air after rinsing with hot water to obtain the rolled hard titanium strip.
The degreasing method combining chemistry and ultrasonic treatment is adopted to remove the rolling oil, so that the degreasing can be ensured to be clean, and the problems of no chromatic aberration, no oxidation and the like on the surface of a finished product are solved.
S104-annealing of finished products: and annealing the rolled hard titanium belt to obtain an annealed titanium belt. Preferably, in this embodiment, a cover annealing process under inert gas protection is adopted in the finished product annealing process, and the specific cover annealing process is as follows: under the protection of inert gas, annealing the titanium strip which is rolled for 8-15 times at the temperature of 400-500 ℃ for 4-6h, and then raising the temperature to 600-650 ℃ for annealing for 8-15 h.
It should be noted that, both the annealing temperature and the annealing speed have certain influence on the processing plasticity of the titanium metal, and the inventors of the present invention have studied the influence of different annealing modes, annealing temperatures and annealing speeds on the processing plasticity of the hot-rolled titanium coil in the first rolling pass and the finished product annealing respectively by using a single-factor variable method, and the results show that: when the continuous annealing process with the temperature of 680-750 ℃ and the speed of 6-15m/min is adopted in the first rolling process rolling procedure, the bulging qualification rate of the produced titanium strip for the bulging of the vacuum cup has more obvious advantages compared with the prior art. And when the finished product annealing process adopts cover annealing under the protection of inert gas, and the specific cover annealing process is as follows: after the titanium belt which is rolled by 8-15 times is annealed for 4-6h at the temperature of 400-500 ℃, and then is heated to 600-650 ℃ for annealing for 8-15h, the bulging qualification rate of the produced titanium belt for the bulging of the vacuum cup is greatly improved. Therefore, in the embodiment, the annealing mode of the first rolling process rolling procedure is preferably continuous annealing, the temperature of the continuous annealing is 680-750 ℃, and the annealing speed is 6-15 m/min; preferably, the annealing mode of the finished product annealing is cover annealing under the protection of inert gas, and the specific cover annealing process comprises the following steps: annealing the titanium belt which is rolled by 8-15 passes at the temperature of 400-500 ℃ for 4-6h, and then heating to the temperature of 600-650 ℃ for annealing for 8-15 h. Meanwhile, in the research process, the following are also found in the embodiment: when the annealing mode of the first rolling process rolling procedure is continuous annealing and the annealing mode of the finished product annealing is cover annealing under the protection of inert gas, compared with the annealing mode with the same first rolling process and finished product annealing, the bulging qualification rate of the produced titanium belt for the bulging of the vacuum cup is obviously improved, and the annealing mode adopting the continuous annealing in the first rolling process rolling and the cover annealing in the finished product annealing has certain synergistic effect.
S105-straightening the titanium strip: and stretching and straightening the annealed titanium belt to prepare a plate with the wave height of less than or equal to 8mm and the arch of less than or equal to 10mm, namely the titanium belt for the bulging of the vacuum cup. Preferably, in the embodiment, a six-roller wet straightening machine is adopted to stretch and straighten the crude titanium strip to prepare the titanium strip for vacuum cup bulging, wherein the width of the titanium strip is 950-1250mm, the wave height of the titanium strip is less than or equal to 8mm, the arch of the titanium strip is less than or equal to 10mm, the thickness of the titanium strip is 0.5-1.0mm, and the thickness precision of the titanium strip is +/-0.01 mm. Wherein the diameters of the bending roll and the leveling roll of the six-roll wet straightening machine are 40mm, and the tension of the straightening machine is 180N/mm2The reduction was 25mm and the speed was 45 m/min.
As can be seen from the above description, in the method for manufacturing a titanium belt for vacuum cup bulging according to this embodiment, after a titanium sponge raw material is made into a slab by combining EB casting and forging, the slab is sequentially subjected to hot rolling, annealing and pickling, cold rolling forming, degreasing treatment combining chemistry and ultrasonic wave, and finished product annealing and straightening treatment, so as to manufacture the titanium belt for vacuum cup bulging. The processing plasticity and extensibility of the titanium belt are modified, so that the prepared titanium belt for the bulging of the vacuum cup has the characteristics of good plasticity, high grain size, uniform rolling performance and good bulging performance. The test result shows that the bulging qualification rate of the titanium belt for bulging the vacuum cup manufactured by the invention can reach more than 97 percent, the multiple bulging treatment is not needed, the problem of orange peel does not occur on the bulging surface, the transverse yield strength is less than or equal to 250Mpa, and the transverse elongation (A) is high50) More than or equal to 35 percent, and the grain size can reach 6 grades and above. In addition, the preparation method of the titanium strip for the bulging of the vacuum cup, provided by the invention, is simple to operate, low in cost and suitable for industrial production.
Embodiments of the present application are described in further detail below with reference to specific examples.
Example 1
The preparation method of the titanium strip for bulging of the vacuum cup provided in this embodiment 1 includes the following steps:
s101, preparing a plate blank: titanium slab is prepared by taking 0A-grade sponge titanium as a raw material through a method combining EB (electron beam) casting and forging. Specifically, an EB furnace is adopted to melt and cast the 0A-level sponge titanium raw material to obtain an ingot with the size specification of 500mm multiplied by 1400 and 1450mm multiplied by L; then, forging the cast ingot by using a 4500-ton forging press to obtain a titanium plate blank with the size specification of 180-; performing machining on the titanium plate blank to obtain two side surface single-side machining amount larger than or equal to 5mm and two large surface single-side machining amount larger than or equal to 7 mm; the integral surface roughness is less than or equal to 6.3um, the whole surface of the plate is exposed to light and the plate shape without oxide skin is remained, and the titanium plate blank for bulging is obtained. The titanium plate blank prepared in the embodiment comprises the following chemical components: more than or equal to 99.6 wt% of Ti, less than or equal to 0.4 wt% of the total impurities, 0.03 wt% of Fe, 0.03 wt% of C, 0.01 wt% of N, 0.006 wt% of H, 0.04 wt% of O and less than or equal to 0.1 wt% of the others; the average particle size of the 0A grade titanium sponge is 3-12.7mm, and the HBW10/1500/30 is not more than 95.
S102-preparing a titanium roll: and (3) carrying out hot rolling on the titanium slab by using a steckel mill according to a conventional method to obtain a hot-rolled titanium coil with the thickness of 4.0mm, and then carrying out continuous pickling annealing on the hot-rolled titanium coil to obtain a pickled hot-rolled titanium coil with the size specification of 4.0 x 1250 x C. Wherein the hot rolling temperature is 860 ℃, and the annealing process is 750 ℃ multiplied by 15 m/min.
S103-cold rolling and forming: and (3) carrying out two-pass (namely a first pass and a second pass) cold rolling on the pickled hot-rolled titanium coil by adopting a 1350mm twenty-roller rolling mill. Wherein the first rolling pass rolling comprises: under the conditions of 4000kN of rolling force and 220N/mm of tension2And rolling the pickled hot-rolled titanium coil for 6 times on the twenty-high rolling mill at the speed of 80m/min, and continuously annealing (the annealing temperature is 750 ℃ and the annealing speed is 15m/min) after rolling to obtain the first rolling process rolled titanium strip with the thickness of 2.0 mm. The second rolling pass comprises: under the conditions of the rolling force of 4000kN and the tension of 180N/mm2And on the twenty-high rolling mill with the speed of 120m/min, carrying out 10-pass rolling on the titanium strip blank rolled in the first rolling process to obtain a titanium strip with the thickness of 0.5mm, the surface roughness of the titanium strip is Ave.0.35um, and the rolling process secondary deformation of the titanium strip is7-15% of the total deformation of the titanium strip, and then removing rolling oil on the surface of the titanium strip by a degreasing method combining chemistry and ultrasonic waves, wherein the degreasing method specifically comprises the following steps:
carrying out alkali liquor soaking treatment on the titanium belt which is rolled for 10 times in the soaking tank, then transferring the titanium belt into the first cleaning tank, and carrying out alkali liquor cleaning under the ultrasonic condition;
carrying out alkali liquor washing treatment on the titanium belt washed by the alkali liquor in the washing tank, and after the alkali liquor washing treatment, transferring the titanium belt into the second washing tank for ultrasonic washing;
and rinsing the ultrasonically washed titanium strip with hot water in the rinsing tank, and drying the titanium strip with hot air after rinsing with hot water to obtain the rolled hard titanium strip.
S104-annealing of finished products: performing coil loosening and argon protection cover annealing on the rolled hard titanium belt to obtain an annealed titanium belt, wherein the cover annealing process comprises the following steps:
and under the protection of argon, annealing the first rolling process rolled titanium strip at the temperature of 450 ℃ for 5 hours, and then heating to 630 ℃ for annealing for 10 hours.
S105-straightening the titanium strip: and stretching and straightening the crude titanium strip by using a six-roller wet straightening machine to prepare the titanium strip for bulging of the vacuum cup, wherein the width of the titanium strip is 1200mm, the wave height of the titanium strip is less than or equal to 8mm, the arch of the titanium strip is less than or equal to 10mm, the thickness of the titanium strip is 0.8mm, and the thickness precision of the titanium strip is +/-0.01 mm. Wherein the diameters of the bending roll and the leveling roll of the six-roll wet straightening machine are 40mm, and the tension of the straightening machine is 180N/mm2The reduction was 25mm and the speed was 45 m/min.
The titanium strip for bulging of the vacuum cup prepared in example 1 was subjected to a performance test, and the results showed that: the transverse tensile strength (sigma b) is 316Mpa, the transverse yield strength (Rp0.2) is 223Mpa, and the elongation after fracture (A50) is 40.5%.
Fig. 2 shows the structure of the titanium strip in the present embodiment under a microscope, and as can be seen from fig. 2, the structure is a uniform equiaxial structure, and has no twinning phenomenon, the grain size reaches 6 levels, which can meet the requirement of high bulging rate of the vacuum cup, and the bulging qualification rate reaches 98.5%.
Example 2
The preparation method of the titanium strip for bulging of the vacuum cup provided in this embodiment 2 specifically includes the following steps:
s101, preparing a plate blank: titanium slab is prepared by taking 0A-grade sponge titanium as a raw material through a method combining EB (electron beam) casting and forging. Specifically, an EB furnace is adopted to melt and cast the 0A-level sponge titanium raw material to obtain an ingot with the size specification of 500mm multiplied by 1400 and 1450mm multiplied by L; then, forging the cast ingot by using a 4500-ton forging press to obtain a titanium plate blank with the size specification of 180-; performing machining on the titanium plate blank to obtain two side surface single-side machining amount larger than or equal to 5mm and two large surface single-side machining amount larger than or equal to 7 mm; the integral surface roughness is less than or equal to 6.3um, and the titanium plate blank for bulging is obtained without leaving oxide skin on the whole surface of the plate. The titanium plate blank prepared in the embodiment comprises the following chemical components: more than or equal to 99.6 wt% of Ti, less than or equal to 0.4 wt% of the total impurities, 0.02 wt% of Fe, 0.03 wt% of C, 0.006 wt% of N, 0.004 wt% of H, 0.05 wt% of O and less than or equal to 0.1 wt% of the rest; the average particle size of the titanium sponge is 3-12.7mm, and the HBW10/1500/30 is not more than 95.
S102-preparing a titanium roll: the titanium slab was hot rolled using a steckel mill according to a conventional method to form a hot rolled titanium coil having a thickness of 4.0mm, and then the hot rolled titanium coil was subjected to continuous pickling annealing to obtain a pickled hot rolled titanium coil having a size specification of 4.0 × 1250 × C. Wherein the hot rolling temperature is 860 ℃, and the annealing process is 750 ℃ multiplied by 15 m/min.
S103-cold rolling and forming: and (3) carrying out two-pass (namely a first pass and a second pass) cold rolling on the pickled hot-rolled titanium coil by adopting a 1350mm twenty-roller rolling mill. Wherein the first rolling pass rolling comprises: under the conditions of 4000kN of rolling force and 220N/mm of tension2And carrying out 7-pass rolling on the pickled hot-rolled titanium coil on the twenty-high rolling mill at the speed of 80m/min, and carrying out continuous annealing (the annealing temperature is 750 ℃ and the annealing speed is 15m/min) after rolling to obtain a first-pass rolled titanium strip with the thickness of 2.0 mm. The second rolling pass comprises: under the conditions of the rolling force of 4000kN and the tension of 180N/mm2And on the twenty-high rolling mill with the speed of 120m/min, the titanium strip blank rolled in the first rolling process is rolled for 13 times to obtain the titanium strip blank with the thickness of 120m/minThe surface roughness of a 0.5mm formed titanium strip is Ave.0.35um, the secondary deformation of a rolling process is 7-15%, the total deformation of the formed titanium strip is 75%, and then rolling oil on the surface of the titanium strip is removed by adopting a degreasing method combining chemistry and ultrasonic waves, wherein the degreasing method specifically comprises the following steps:
carrying out alkali liquor soaking treatment on the titanium belt subjected to 13-pass rolling in the soaking tank, then transferring the titanium belt into the first cleaning tank, and carrying out alkali liquor cleaning under the ultrasonic condition;
carrying out alkali liquor washing treatment on the titanium belt washed by the alkali liquor in the washing tank, and after the alkali liquor washing treatment, transferring the titanium belt into the second washing tank for ultrasonic washing;
and rinsing the ultrasonically washed titanium strip with hot water in the rinsing tank, and drying the titanium strip with hot air after rinsing with hot water to obtain the rolled hard titanium strip.
S104-annealing of finished products: and performing cover annealing under inert gas protection on the rolled hard titanium belt to obtain an annealed titanium belt, wherein the cover annealing process comprises the following steps:
and under the protection of inert gas, annealing the first rolling process rolled titanium strip at the temperature of 450 ℃ for 5h, and then raising the temperature to 630 ℃ for annealing for 10 h.
S105-straightening the titanium strip: and stretching and straightening the crude titanium strip by using a six-roller wet straightening machine to prepare the titanium strip for bulging of the vacuum cup, wherein the width of the titanium strip is 1200mm, the wave height of the titanium strip is less than or equal to 8mm, the arch of the titanium strip is less than or equal to 10mm, the thickness of the titanium strip is 0.8mm, and the thickness precision of the titanium strip is +/-0.01 mm. Wherein the diameters of the bending roll and the leveling roll of the six-roll wet straightening machine are 40mm, and the tension of the straightening machine is 180N/mm2The reduction was 25mm and the speed was 45 m/min.
The titanium strip for bulging of the vacuum cup prepared in example 1 was subjected to a performance test, and the results showed that: the transverse tensile strength (sigma b) is 326MPa, the transverse yield strength (Rp0.2) is 242MPa, and the elongation after fracture (A50) is 30.8%.
Fig. 3 shows the structure of the titanium strip under the microscope in this embodiment, as can be seen from fig. 3, the structure is a uniform equiaxial structure, and has no twinning phenomenon, the grain size reaches 8 level, the requirement of high bulging rate of the vacuum cup can be met, and the bulging qualification rate reaches 97.1%.
Example 3
This example 3 provides, as a comparative example to examples 1 to 2, a method for producing a titanium ribbon for cup bulging, comprising the steps of:
s101, preparing a plate blank: titanium slab is prepared by taking 0A-grade sponge titanium as a raw material through a method combining EB (electron beam) casting and forging. Specifically, an EB furnace is adopted to melt and cast the 0A-level sponge titanium raw material to obtain an ingot with the size specification of 500mm multiplied by 1400 and 1450mm multiplied by L; then, forging the cast ingot by using a 4500-ton forging press to obtain a titanium plate blank with the size specification of 180-; performing machining on the titanium plate blank to obtain two side surface single-side machining amount larger than or equal to 5mm and two large surface single-side machining amount larger than or equal to 7 mm; the integral surface roughness is less than or equal to 6.3um, the whole surface of the plate is exposed to light and the plate shape without oxide skin is remained, and the titanium plate blank for bulging is obtained. The titanium plate blank prepared in the embodiment comprises the following chemical components: more than or equal to 99.6 wt% of Ti, less than or equal to 0.4 wt% of the total impurities, 0.02 wt% of Fe, 0.03 wt% of C, 0.006 wt% of N, 0.004 wt% of H, 0.045 wt% of O and less than or equal to 0.1 wt% of the rest; the average granularity of the 0A-grade titanium sponge is 3-12.7 mm.
S102-preparing a titanium roll: the titanium slab was hot rolled using a steckel mill according to a conventional method to form a hot rolled titanium coil having a thickness of 4.0mm, and then the hot rolled titanium coil was subjected to continuous pickling annealing to obtain a pickled hot rolled titanium coil having a size specification of 4.0 × 1250 × C. Wherein the hot rolling temperature is 860 ℃, and the annealing process is 750 ℃ multiplied by 15 m/min.
S103-cold rolling and forming: and (3) carrying out two-rolling process (namely a first rolling process and a second rolling process) cold rolling on the pickled hot-rolled titanium coil. Wherein the first rolling pass rolling comprises: the rolling force of the twenty-high roll mill is 4000kN, and the tension is 220N/mm2And carrying out 7-pass rolling on the pickled hot-rolled titanium coil under the condition of the speed of 80m/min, and carrying out continuous annealing (the annealing temperature is 750 ℃ and the annealing speed is 15m/min) after the rolling to obtain a first-pass rolled titanium belt with the thickness of 2.0 mm. The second rolling pass comprises: under the conditions of the rolling force of 4000kN and the tension of 180N/mm2Rolling the first rolling pass of the pair on the twenty-high rolling mill with the speed of 120m/minCarrying out 13-pass rolling on the titanium strip to obtain a formed titanium strip with the thickness of 0.5mm, wherein the surface roughness of the formed titanium strip is Ave.0.35um, the secondary deformation of the rolling process is 7-15%, and the total deformation of the formed titanium strip is 75%, and then removing rolling oil on the surface of the titanium strip by adopting a degreasing method combining chemistry and ultrasonic waves, wherein the method specifically comprises the following steps:
carrying out alkali liquor soaking treatment on the titanium belt subjected to 13-pass rolling in the soaking tank, then transferring the titanium belt into the first cleaning tank, and carrying out alkali liquor cleaning under the ultrasonic condition;
carrying out alkali liquor washing treatment on the titanium belt washed by the alkali liquor in the washing tank, and after the alkali liquor washing treatment, transferring the titanium belt into the second washing tank for ultrasonic washing;
and rinsing the ultrasonically washed titanium strip with hot water in the rinsing tank, and drying the titanium strip with hot air after rinsing with hot water to obtain the rolled hard titanium strip.
S104-annealing of finished products: and continuously annealing the rolled hard titanium strip, wherein the annealing processes are respectively as follows: 10m/min at 820 ℃; 820 ℃ multiplied by 8m/min, 820 ℃ multiplied by 6m/min, 820 ℃ multiplied by 4m/min, 820 ℃ multiplied by 2m/min and the heat preservation time is 10 h).
S105-straightening the titanium strip: and stretching and straightening the crude titanium strip by using a six-roller wet straightening machine to prepare the titanium strip for bulging of the vacuum cup, wherein the width of the titanium strip is 1200mm, the wave height of the titanium strip is less than or equal to 8mm, the arch of the titanium strip is less than or equal to 10mm, the thickness of the titanium strip is 0.8mm, and the thickness precision of the titanium strip is +/-0.01 mm. Wherein the diameters of the bending roll and the leveling roll of the six-roll wet straightening machine are 40mm, and the tension of the straightening machine is 180N/mm2The reduction was 25mm and the speed was 45 m/min.
The titanium tape for bulging of the vacuum cup prepared in example 3 was subjected to a performance test, and the results are shown in table 2.
TABLE 2 titanium strip Performance test results under different annealing Processes
As can be seen from table 2, in the process of preparing the titanium strip for bulging of the vacuum cup by using the continuous annealing process, when the continuous annealing is used in the product annealing process, although the strength and the grain size of the titanium strip product are improved, the bulging yield is obviously reduced, and particularly when the annealing process of 820 ℃ x 6-10m/min is used, the bulging requirement of the vacuum cup cannot be met, and the bulging cracks. Therefore, the embodiment of the application adopts continuous annealing in the hot rolling and the first rolling process rolling, and adopts cover annealing in the finished product annealing process to obviously improve the bulging yield.
According to the embodiment, the titanium plate blank components provided by the embodiment of the application are the optimal range of the bulging of the vacuum cup, and if the content of each chemical component exceeds the range, the strength of the titanium belt finished product is increased, the shaping is reduced, the bulging fracture is easy to occur, and the yield is reduced. Meanwhile, the cold rolling process adopts two-rolling-process cold rolling forming, and the deformation amount and the annealing temperature of the finished product in the rolling process are strictly controlled, so that the problems of large structure, uneven grain size and no twin crystal caused by overlarge deformation amount and overhigh annealing temperature and rough bulging surface are effectively avoided. According to the method, the titanium belt with the optimal bulging property is prepared by controlling parameters from the components of the plate blank to the processing process and comprehensively considering the shaping, microstructure and size control of the titanium belt.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. A preparation method of a titanium strip for vacuum cup bulging is characterized by comprising the following steps:
preparing a plate blank: performing EB (electron beam) casting on a titanium sponge raw material, and forging a formed cast ingot to obtain a titanium slab;
preparing a titanium coil: carrying out hot rolling on the titanium plate blank to obtain a hot-rolled titanium coil, and carrying out annealing and acid pickling on the hot-rolled titanium coil;
cold rolling and forming: carrying out cold rolling on the pickled hot-rolled titanium coil, and carrying out chemical and ultrasonic combined degreasing treatment after the cold rolling to obtain a rolled hard titanium strip;
annealing of a finished product: annealing the rolled hard titanium belt to obtain an annealed titanium belt;
straightening the titanium belt: and straightening the annealed titanium belt to prepare a plate with the wave height of less than or equal to 8mm and the arch of less than or equal to 10mm, thus obtaining the titanium belt for the bulging of the vacuum cup.
2. A method for producing a titanium strip for cup bulging as set forth in claim 1, wherein said cold roll forming includes a first rolling pass rolling and a second rolling pass rolling;
the first rolling pass rolling comprises: at 200-2Under the tension of the steel strip, carrying out 5-7 times of rolling on the pickled hot-rolled titanium coil, and carrying out annealing pickling after rolling to obtain a first rolling process rolled titanium strip;
the second rolling pass comprises: at 160-2Under the tension of the first rolling process, rolling the titanium strip rolled by the first rolling process for 8-15 times, and performing chemical and ultrasonic combined degreasing treatment after rolling to obtain the rolled hard titanium strip.
3. The method for preparing a titanium strip for cup bulging according to claim 2, wherein the degreasing treatment by combination of chemical and ultrasonic waves comprises:
carrying out alkali liquor soaking treatment on the titanium belt obtained by 8-15 passes of rolling, and then carrying out alkali liquor cleaning under the ultrasonic condition;
carrying out alkali liquor washing treatment on the titanium belt washed by the alkali liquor, and carrying out ultrasonic water washing after the alkali liquor washing treatment;
and rinsing the titanium strip subjected to ultrasonic water washing with hot water, and drying the titanium strip with hot air after rinsing with hot water to obtain the rolled hard titanium strip.
4. The method for preparing the titanium strip for cup bulging according to claim 2, wherein the pass deformation of the first rolling pass is 7-20%, and the total deformation of the hot-rolled titanium coil in the first rolling pass is not less than 40%.
5. The method for preparing the titanium strip for cup bulging as claimed in claim 4, wherein the annealing manner of the first rolling is continuous annealing, the temperature of the continuous annealing is 680-750 ℃, and the speed is 6-15 m/min.
6. The method for preparing the titanium strip for cup bulging according to claim 2, wherein the pass deformation of the second rolling pass is 5-17%, and the total deformation of the titanium strip blank rolled by the first rolling pass in the second rolling pass is greater than or equal to 50%.
7. The method for preparing a titanium strip for cup bulging according to claim 2, wherein the annealing manner in the finished product annealing process is inert gas shielded hood annealing, and the hood annealing comprises:
under the protection of inert gas, annealing the hard titanium rolling strip at the temperature of 400-500 ℃ for 4-6h, and then heating to the temperature of 600-650 ℃ for annealing for 8-15 h.
8. The method for manufacturing a titanium strip for vacuum cup bulging as set forth in claim 1, wherein the titanium sponge raw material has a particle size of 3-12.7mm and HBW10/1500/30 is not more than 95.
9. The method of manufacturing a titanium strip for cup bulging according to claim 8, wherein the manufacturing of the slab includes:
performing EB fusion casting on the titanium sponge raw material to obtain 500mm & ltx & gt 1400 & lt- & gt 1450mm & ltx & gt L ingot casting, forging the ingot casting by using a forging press to obtain 180 mm & ltx & gt 950 & lt- & gt 1250mm & ltx & gt L titanium plate blanks, and performing machining on the titanium plate blanks to obtain titanium plate blanks with the processing amount of single surfaces of two side surfaces being more than or equal to 5mm, the processing amount of single surfaces of two large surfaces being more than or equal to 7mm, the integral surface roughness being less than or equal to 6.3 mu m, and the whole surfaces being exposed to light and free of oxide skin.
10. The method for preparing a titanium strip for cup bulging according to claim 9, wherein the prepared titanium plate blank comprises the following chemical components:
ti is more than or equal to 99.6 wt%; and impurities
Fe is less than or equal to 0.05 wt%, C is less than or equal to 0.03 wt%, N is less than or equal to 0.01 wt%, H is less than or equal to 0.006 wt%, O is less than or equal to 0.06 wt%, others are less than or equal to 0.1 wt%, and the total amount of impurities is less than or equal to 0.4 wt%.
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| (美)乔治·E.陶敦编；叶卫平译: "美国金属学会热处理手册 E卷 非铁合金的热处理", 四川科学技术出版社, pages: 608 - 80 * |
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| CN114405995A (en) * | 2021-12-13 | 2022-04-29 | 新疆湘润新材料科技有限公司 | Preparation method of wide pure titanium foil coiled strip |
| CN114405995B (en) * | 2021-12-13 | 2023-12-29 | 新疆湘润新材料科技有限公司 | Preparation method of wide pure titanium foil tape |
| CN114395712A (en) * | 2021-12-31 | 2022-04-26 | 湖南湘投金天钛金属股份有限公司 | Titanium coil for deep drawing, preparation method thereof and titanium product |
| CN114395712B (en) * | 2021-12-31 | 2023-02-03 | 湖南湘投金天钛金属股份有限公司 | Titanium coil for deep drawing, preparation method thereof and titanium product |
| CN115323137A (en) * | 2022-03-16 | 2022-11-11 | 西安庄信新材料科技有限公司 | Preparation method of titanium plate for architectural decoration |
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