CN105170686A - Processing method for high-purity titanium sheet for coating titanium anode base material - Google Patents
Processing method for high-purity titanium sheet for coating titanium anode base material Download PDFInfo
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- CN105170686A CN105170686A CN201510428749.0A CN201510428749A CN105170686A CN 105170686 A CN105170686 A CN 105170686A CN 201510428749 A CN201510428749 A CN 201510428749A CN 105170686 A CN105170686 A CN 105170686A
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Abstract
Provided is a processing method for a high-purity titanium sheet for a coating titanium anode base material. O-stage sponge titanium with the average particle size being 3-25.4 mm is placed in an electron beam cold hearth and melted in a vacuum state so that a high-purity titanium slab can be obtained through purification; a hot coil which is 2.5-5 mm thick is manufactured through rolling of a steckel mill, and annealing is performed; shot blasting and pickling treatment need to be performed after annealing; the hot coil is placed on a reversible cold rolling machine to be subjected to many times of rolling; finally, a cold coil which is 0.5-2 mm thick can be obtained; the deformation rate is controlled to be 40-60% during each time of rolling; then the cold coil is subjected to degreasing treatment; then complete recrystallization annealing is performed in the vacuum state or the argon protection state, wherein the annealing temperature is controlled to be 600-720 DEG C and a titanium coil is obtained. As is detected, the average grain size of the titanium is controlled to be 15-30 microns, and the high-purity titanium sheet for the coating titanium anode base material is obtained after the titanium coil is straightened. The unevenness of the high-purity titanium sheet is smaller than or equal to 3 mm/m, and no strip-shaped flow direction lines exist after the high-purity titanium sheet is used as a coating.
Description
Technical field
The invention belongs to Rare Metals Materials processing technique field, refer more particularly to a kind of processing method of coating titanium anode high-purity titanium thin plate.
Background technology
Coating titanium anode is mainly used in electrochemistry and electrometallurgy Liang Ge department.In electrochemical process, Ni―Ti anode has good corrosion resistance, higher catalytic activity, can keep the stable of size and profile, be widely used in the fields such as plating, wastewater treatment, Organic electro-synthesis, cathodic protection and chlorine industry in electrolytic process.
Pure titanium generally selected by coating titanium anode base material, and require that material purity at least reaches TA1 standard, if the base material purity used is inadequate, decay resistance will be had a greatly reduced quality, antianode also has a great impact service life, and because coating titanium anode raw materials is expensive, preparation cost is higher, and be generally 1 ~ 2 year service life, add the operation cost of relevant enterprise.
Coating titanium anode base material high purity titanium thin slab technique requires very high, and production difficulty is very big, especially for high-end fields such as plating, some requirement titanium plate quality purities reach more than 99.9%, because the purity of base material titanium plate is higher, decay resistance is better, and service life is longer.In addition its coating layer thickness distribution that titanium lath particle size difference is less is also comparatively even, suitable grain size range, and crystal grain orientation distribution is even, and coating rear surface coating does not allow to occur that strip flows to line.
Improving the stability of high purity titanium thin plate, increasing the service life is one of the emphasis direction of this area research.
Summary of the invention
For above-mentioned the deficiencies in the prior art; the invention provides a kind of processing method of coating titanium anode base material high purity titanium thin plate; its quality purity of high purity titanium thin plate that this processing method is produced is not less than 99.9%; unevenness is not more than 3mm/m; average crystal grain particle diameter 15 ~ 30 μm; the size of crystal grain and orientation distribution are comparatively even, meet high-end coatings Ni―Ti anode base material associated specifications, can be widely used in the fields such as plating, wastewater treatment, Organic electro-synthesis, cathodic protection and chlorine industry.
In order to realize foregoing invention object, the present invention adopts following technical scheme:
A kind of processing method of coating titanium anode base material high purity titanium thin plate; this processing method comprises slab preparation, hot rolling preparation, cold coiling preparation, annealing, straightener aligning or stretch-bending straightening five processes; wherein slab preparation process uses electron-beam cold bed furnace or VAR stove; hot rolling preparation process uses steekle mill or continuous hot-rolling mill; cold coiling preparation process uses reversable cold-rolling machine or tandem mills; annealing process uses vacuum or argon shield state, and each process is described below:
Prepared by slab: 1. select and meet standard GB/T/T2524-2010 and product grade is the titanium sponge of MHT-95, titanium sponge rank is not less than O level, 2. from above-mentioned 1. optimize the titanium sponge that average crystal grain particle diameter is 3 ~ 25.4mm, titanium sponge be placed in electron-beam cold bed furnace or VAR stove and under vacuum conditions its melting purified, Fe≤0.03% in titanium sponge after stokehold testing requirement is purified, O≤0.07%, N≤0.01%, high-purity titanium slab is obtained after coming out of the stove, described high-purity titanium slab need process through milling face, during the process of milling face, the thickness in one side milling face can not be less than 4mm, again GD-MS elementary analysis is carried out to described high-purity titanium slab after the process of milling face, require that the quality purity of Ti in described high-purity titanium slab requires to reach more than 99.9%,
Prepared by hot rolling: the hot rolling 3. above-mentioned 2. described high-purity titanium slab being rolled into 2.5 ~ 5mm thickness by steekle mill or continuous hot-rolling mill, be placed in continuous annealing furnace by described hot rolling and anneal, after annealing, the surface of described hot rolling need through ball blast and pickling processes;
Prepared by cold coiling: 4. above-mentioned 3. described hot rolling is placed on reversable cold-rolling machine or tandem mills carries out multi-pass rolling, the cold coiling of final acquisition 0.5 ~ 2.0mm thickness, the deformation rate of every time rolling controls 40 ~ 60%, the thickness setting above-mentioned 3. described hot rolling is Amm and the thickness of described cold coiling after every time rolling is Bmm, then the deformation rate of every time rolling equals [A-B}/A] × 100%;
Annealing: 5. first ungrease treatment is carried out to above-mentioned 4. described cold coiling, then under vacuum or argon shield state, perfect recrystallization annealing is carried out, the temperature of recrystallization annealing controls at 600 ~ 720 DEG C, obtain titanium volume after recrystallization annealing, the average grain size of described titanium volume requires to control at 15 ~ 30 μm after testing;
Straightener aligning or stretch-bending straightening: 6. utilize straightener aligning or stretch bending to rectify unit and row straightening processing is involved in above-mentioned 5. described titanium and obtains coating titanium anode base material high purity titanium thin plate, require the unevenness≤3mm/m of this high purity titanium thin plate.
Owing to adopting technical scheme described above, the present invention produces following good effect:
1. the preferred purity of the present invention is not less than the titanium sponge of O level and carries out postsearch screening to it, and the electron-beam cold bed furnace melting be mingled with by effectively removing high density obtains high-purity titanium slab, and the quality purity of high-purity titanium slab can reach more than 99.9%.
2. processing method Absorbable organic halogens of the present invention produces coating titanium anode base material high purity titanium thin plate, and evenly, the average diameter of crystal grain reaches 15 ~ 30 μm, there is not strip and flow to line after coating for the grain size of this high purity titanium thin plate and orientation.
Detailed description of the invention
The present invention is a kind of processing method of coating titanium anode base material high purity titanium thin plate, its quality purity of high purity titanium thin plate that this processing method is produced is not less than 99.9%, unevenness is not more than 3mm/m, average crystal grain particle diameter 15 ~ 30 μm, the size of crystal grain and orientation distribution are comparatively even, meet high-end coatings Ni―Ti anode base material associated specifications.
Processing method of the present invention comprises slab preparation, prepared by hot rolling, prepared by cold coiling, annealing, straightener aligning or stretch-bending straightening five processes, wherein slab preparation process uses electron-beam cold bed furnace or VAR stove, hot rolling preparation process uses steekle mill or continuous hot-rolling mill, cold coiling preparation process uses reversable cold-rolling machine or tandem mills, annealing process uses vacuum or argon shield state, part of not stating in above-mentioned five processes is routine techniques, routine techniques+described technical scheme is necessary requirement of the present invention, therefore about the content of routine techniques is not repeating.
In slab preparation process:
1. select and meet standard GB/T/T2524-2010 and product grade is the titanium sponge of MHT-95, titanium sponge rank is not less than O level.
2. from above-mentioned 1. optimize the titanium sponge that average crystal grain particle diameter is 3 ~ 25.4mm, preferred process is also the process of postsearch screening, titanium sponge be placed in electron-beam cold bed furnace or VAR stove and under vacuum conditions its melting purified, Fe≤0.03% in titanium sponge after stokehold testing requirement is purified, O≤0.07%, N≤0.01%, high-purity titanium slab is obtained after coming out of the stove, described high-purity titanium slab need process through milling face, during the process of milling face, the thickness in one side milling face can not be less than 4mm, again GD-MS elementary analysis is carried out to described high-purity titanium slab after the process of milling face, require that the quality purity of Ti in described high-purity titanium slab requires to reach more than 99.9%.
In hot rolling preparation process:
3. above-mentioned 2. described high-purity titanium slab is rolled into the hot rolling of 2.5 ~ 5mm thickness by steekle mill or continuous hot-rolling mill, described hot rolling is placed in continuous annealing furnace and anneals, this annealing process can make described hot rolling obtain first time recrystallized structure, and after annealing, the surface of described hot rolling need through ball blast and pickling processes.
In cold coiling preparation process:
4. above-mentioned 3. described hot rolling is placed on reversable cold-rolling machine or tandem mills carries out multi-pass rolling, the cold coiling of final acquisition 0.5 ~ 2.0mm thickness, the deformation rate of every time rolling controls 40 ~ 60%, the thickness setting above-mentioned 3. described hot rolling is Amm and the thickness of described cold coiling after every time rolling is Bmm, then the deformation rate of every time rolling equals [A-B}/A] × 100%.
Attention: when deformation rate≤40%; the crystal grain of described cold coiling can be out of shape and broken insufficient; add that the minute quantity of impurity element exists; hinder the ability of the migration of the crystal boundary of titanium crystal grain material more weak; so just be not easy to suppress growing up of crystal grain, after easily causing second time recrystallization annealing, described titanium volume size of microcrystal is uneven.When deflection >=60%, Titanium can produce obvious anisotropy when cold roller and deformed, and after second time recrystallization annealing, the too small or local grain phenomenon bigger than normal of crystal grain easily appears in described titanium volume.
In annealing process: 5. first ungrease treatment is carried out to above-mentioned 4. described cold coiling, then under vacuum or argon shield state, second time recrystallization annealing is carried out, the temperature of second time recrystallization annealing controls at 600 ~ 720 DEG C, titanium volume is obtained after second time recrystallization annealing, the average grain size of described titanium volume requires to control at 15 ~ 30 μm after testing, after second time recrystallization annealing, the crystal grain distribution of described titanium volume detects through metallographic and does not present size non-uniform phenomenon, if the crystal grain of described titanium volume presents size non-uniform phenomenon, then described titanium twists in galvanization process and very easily occurs that titanium is leaked namely without coating phenomenon in local.
In straightener aligning or stretch-bending straightening process:
6. utilize straightener aligning or stretch bending to rectify unit involve in row straightening processing to above-mentioned 5. described titanium and obtain coating titanium anode base material high purity titanium thin plate, require the unevenness≤3mm/m of this high purity titanium thin plate, the size required for coating titanium anode base material after cutting, can be obtained.
Claims (1)
1. the coating titanium anode base material processing method of high purity titanium thin plate; this processing method comprises slab preparation, hot rolling preparation, cold coiling preparation, annealing, straightener aligning or stretch-bending straightening five processes; wherein slab preparation process uses electron-beam cold bed furnace or VAR stove; hot rolling preparation process uses steekle mill or continuous hot-rolling mill; cold coiling preparation process uses reversable cold-rolling machine or tandem mills; annealing process uses vacuum or argon shield, it is characterized in that:
Prepared by slab: 1. select and meet standard GB/T/T2524-2010 and product grade is the titanium sponge of MHT-95, titanium sponge rank is not less than O level, 2. from above-mentioned 1. optimize the titanium sponge that average crystal grain particle diameter is 3 ~ 25.4mm, titanium sponge be placed in electron-beam cold bed furnace or VAR stove and under vacuum conditions its melting purified, Fe≤0.03% in titanium sponge after stokehold testing requirement is purified, O≤0.07%, N≤0.01%, high-purity titanium slab is obtained after coming out of the stove, described high-purity titanium slab need process through milling face, during the process of milling face, the thickness in one side milling face can not be less than 4mm, again GD-MS elementary analysis is carried out to described high-purity titanium slab after the process of milling face, require that the quality purity of Ti in described high-purity titanium slab requires to reach more than 99.9%,
Prepared by hot rolling: the hot rolling 3. above-mentioned 2. described high-purity titanium slab being rolled into 2.5 ~ 5mm thickness by steekle mill or continuous hot-rolling mill, be placed in continuous annealing furnace by described hot rolling and anneal, after annealing, the surface of described hot rolling need through ball blast and pickling processes;
Prepared by cold coiling: 4. above-mentioned 3. described hot rolling is placed on reversable cold-rolling machine or tandem mills carries out multi-pass rolling, the cold coiling of final acquisition 0.5 ~ 2.0mm thickness, the deformation rate of every time rolling controls 40 ~ 60%, the thickness setting above-mentioned 3. described hot rolling is Amm and the thickness of described cold coiling after every time rolling is Bmm, then the deformation rate of every time rolling equals [A-B}/A] × 100%;
Annealing: 5. first ungrease treatment is carried out to above-mentioned 4. described cold coiling, then under vacuum or argon shield state, perfect recrystallization annealing is carried out, the temperature of recrystallization annealing controls at 600 ~ 720 DEG C, obtain titanium volume after recrystallization annealing, the average grain size of described titanium volume requires to control at 15 ~ 30 μm after testing;
Straightener aligning or stretch-bending straightening: 6. utilize straightener aligning or stretch bending to rectify unit and row straightening processing is involved in above-mentioned 5. described titanium and obtains coating titanium anode base material high purity titanium thin plate, require the unevenness≤3mm/m of this high purity titanium thin plate.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105887133A (en) * | 2016-06-28 | 2016-08-24 | 湖南新发科技有限责任公司 | Method for preparing high-deformation resistance titanium anode from electrolytic manganese dioxide |
| CN106544544A (en) * | 2016-12-06 | 2017-03-29 | 青海聚能钛业股份有限公司 | A kind of method of electron-beam cold bed furnace single melting TC4 titan alloy casting ingots |
| CN109030130A (en) * | 2017-06-08 | 2018-12-18 | 宁波江丰电子材料股份有限公司 | Titanium crystalline substance sample preparation methods and titanium crystalline substance sample for GDMS detection |
| CN109530438A (en) * | 2018-11-07 | 2019-03-29 | 湖北第二师范学院 | A kind of light radiation the space pure titanium strip in razor-thin of Zn-Ag composite deposite and its production method |
| CN109797313A (en) * | 2018-12-19 | 2019-05-24 | 洛阳双瑞精铸钛业有限公司 | A kind of cookware punching press titanium volume and preparation method thereof |
| CN110724834A (en) * | 2019-10-18 | 2020-01-24 | 洛阳双瑞精铸钛业有限公司 | TA2 hot-rolled pure titanium plate preparation method based on oxygen equivalent annealing process |
| CN110935726A (en) * | 2019-11-26 | 2020-03-31 | 陕西凸鹏钛锆股份有限公司 | Continuous rolling solution treatment process for TC4 titanium alloy strip |
| CN112048691A (en) * | 2020-09-18 | 2020-12-08 | 安徽工业大学 | Method for preparing face-centered cubic phase in high-purity titanium thin strip |
| CN113948721A (en) * | 2021-09-08 | 2022-01-18 | 洛阳双瑞精铸钛业有限公司 | Preparation method of titanium metal bipolar plate substrate of hydrogen fuel cell |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105887133A (en) * | 2016-06-28 | 2016-08-24 | 湖南新发科技有限责任公司 | Method for preparing high-deformation resistance titanium anode from electrolytic manganese dioxide |
| CN106544544A (en) * | 2016-12-06 | 2017-03-29 | 青海聚能钛业股份有限公司 | A kind of method of electron-beam cold bed furnace single melting TC4 titan alloy casting ingots |
| CN106544544B (en) * | 2016-12-06 | 2018-08-10 | 青海聚能钛业股份有限公司 | A kind of method of electron-beam cold bed furnace single melting TC4 titan alloy casting ingots |
| CN109030130A (en) * | 2017-06-08 | 2018-12-18 | 宁波江丰电子材料股份有限公司 | Titanium crystalline substance sample preparation methods and titanium crystalline substance sample for GDMS detection |
| CN109530438A (en) * | 2018-11-07 | 2019-03-29 | 湖北第二师范学院 | A kind of light radiation the space pure titanium strip in razor-thin of Zn-Ag composite deposite and its production method |
| CN109797313A (en) * | 2018-12-19 | 2019-05-24 | 洛阳双瑞精铸钛业有限公司 | A kind of cookware punching press titanium volume and preparation method thereof |
| CN110724834A (en) * | 2019-10-18 | 2020-01-24 | 洛阳双瑞精铸钛业有限公司 | TA2 hot-rolled pure titanium plate preparation method based on oxygen equivalent annealing process |
| CN110724834B (en) * | 2019-10-18 | 2021-12-17 | 洛阳双瑞精铸钛业有限公司 | TA2 hot-rolled pure titanium plate preparation method based on oxygen equivalent annealing process |
| CN110935726A (en) * | 2019-11-26 | 2020-03-31 | 陕西凸鹏钛锆股份有限公司 | Continuous rolling solution treatment process for TC4 titanium alloy strip |
| CN110935726B (en) * | 2019-11-26 | 2021-03-16 | 陕西凸鹏钛锆股份有限公司 | Continuous rolling solution treatment process for TC4 titanium alloy strip |
| CN112048691A (en) * | 2020-09-18 | 2020-12-08 | 安徽工业大学 | Method for preparing face-centered cubic phase in high-purity titanium thin strip |
| CN113948721A (en) * | 2021-09-08 | 2022-01-18 | 洛阳双瑞精铸钛业有限公司 | Preparation method of titanium metal bipolar plate substrate of hydrogen fuel cell |
| WO2023036206A1 (en) * | 2021-09-08 | 2023-03-16 | 洛阳双瑞精铸钛业有限公司 | Preparation method for titanium metal bipolar plate substrate of hydrogen fuel cell |
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Application publication date: 20151223 |