CN110923597A - Vacuum annealing treatment process for titanium strip coil - Google Patents

Vacuum annealing treatment process for titanium strip coil Download PDF

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Publication number
CN110923597A
CN110923597A CN201911223122.6A CN201911223122A CN110923597A CN 110923597 A CN110923597 A CN 110923597A CN 201911223122 A CN201911223122 A CN 201911223122A CN 110923597 A CN110923597 A CN 110923597A
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China
Prior art keywords
titanium
strip coil
titanium strip
coil
water
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Pending
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CN201911223122.6A
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Chinese (zh)
Inventor
侯军涛
郭磊
鲁毅
王尧
任怀智
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Xi'an Zhuang Xinxin Mstar Technology Ltd
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Xi'an Zhuang Xinxin Mstar Technology Ltd
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Priority to CN201911223122.6A priority Critical patent/CN110923597A/en
Publication of CN110923597A publication Critical patent/CN110923597A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing 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
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/026Anodisation with spark discharge
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon

Abstract

The invention discloses a titanium strip coil vacuum annealing treatment process, which comprises the following specific treatment process steps: the method comprises the following steps: putting titanium ingots and leftover bits and pieces into a titanium melting furnace, converting the solid titanium ingots into liquid titanium water, and standing and preserving the temperature of the titanium water; step two: allowing the titanium water after standing and heat preservation to flow into a casting and rolling machine through a pipeline, cooling by circulating water while flowing in, and continuously casting and rolling from the casting and rolling machine and then curling to obtain a titanium strip coil; step three: removing oxide skin on the surface of the hot coil from the titanium strip coil obtained in the step two by adopting shot blasting and acid washing, and quickly drying by adopting an industrial hot air blower after cleaning; step four: and on the basis of the third step, arc discharge is generated in the prepared electrolyte by utilizing a micro-arc oxidation technology, and the ceramic coating is obtained by in-situ growth on the metal surface of the cleaned and dried titanium strip coil. The titanium strip coil treatment process is stable and reliable, simple in equipment, convenient to operate, strong in practicability and suitable for wide popularization and use.

Description

Vacuum annealing treatment process for titanium strip coil
Technical Field
The invention belongs to the technical field of titanium strip coil production, and particularly relates to a vacuum annealing treatment process for a titanium strip coil.
Background
The induction heating method in the titanium strip coil heating and annealing device is a mature technology and is feasible in principle. However, the efficiency is low, the use is inconvenient, and the method of direct heating by induction vacuum is used for the vacuum annealing of the titanium coil, which is a brand new idea compared with the traditional method of heating and annealing the titanium coil, and needs to design brand new equipment and process. However, the surface of the titanium strip coil produced by the existing induction vacuum direct heating method is not smooth enough, cannot be in the natural color of metal, and has the defects of oxide skin and the like, and the produced titanium strip coil has the defects of unobvious anti-crack anticorrosion effect on the surface, low efficiency and poor practicability.
Disclosure of Invention
The invention aims to provide a titanium strip coil vacuum annealing treatment process, which aims to solve the problems that the surface of a titanium strip coil produced by the existing induction vacuum direct heating method is not smooth enough, cannot be in the natural color of metal, has the defects of oxide skin and the like, and the produced titanium strip coil has an unobvious anti-crack anticorrosion effect on the surface, low efficiency and poor practicability.
In order to achieve the purpose, the invention provides the following technical scheme: a titanium strip coil vacuum annealing treatment process comprises the following specific treatment process steps:
the method comprises the following steps: putting titanium ingots and leftover bits and pieces into a titanium melting furnace, converting the solid titanium ingots into liquid titanium water, and standing and preserving the temperature of the titanium water;
step two: allowing the titanium water after standing and heat preservation to flow into a casting and rolling machine through a pipeline, cooling by circulating water while flowing in, and continuously casting and rolling from the casting and rolling machine and then curling to obtain a titanium strip coil;
step three: removing oxide skin on the surface of the hot coil from the titanium strip coil obtained in the step two by adopting shot blasting and acid washing, and quickly drying by adopting an industrial hot air blower after cleaning;
step four: arc discharge is generated in the prepared electrolyte by utilizing the micro-arc oxidation technology on the basis of the third step, and a ceramic coating is obtained by in-situ growth on the metal surface of the cleaned and dried titanium strip coil;
step five: placing the titanium strip coil into an annealing furnace, purging the annealing furnace by using inert gas to completely replace the atmosphere in the annealing furnace, heating the titanium strip coil to 400-450 ℃ at a heating speed of 55-170 ℃/h, and preserving heat for 22-24 h;
step six: vacuumizing the annealing furnace to 10-4 Pa of vacuum degree; removing air, replacing the air with argon in the air removing process, and performing forced circulation through a fan to uniformly cool the air to 120-150 ℃ at a cooling speed of 5 ℃/h;
step seven: and (3) carrying out vacuum exhaust in the annealing furnace until the pressure is 3-5 multiplied by 10 < -2 > Pa, and then cooling to room temperature at the speed of 5-10 ℃/min to take out the titanium strip coil.
Further, the electrolyte prepared in the fourth step is one of commonly used Na2SO4, Na2CO3, Na2SiO3 and Na3PO 4.
Further, in the third step, the granularity of the steel shot is 0.20-0.40 mm, the hardness of the steel shot is 50-55 HV, the projection speed is as follows: 55-70 m/s, projection density: 75-95 kg/m2, acid pickling for dephosphorization, using a mixed solution of 15-25% of nitric acid and 4-8% of hydrofluoric acid to carry out acid pickling for dephosphorization on the hot-rolled titanium coil, controlling the acid pickling temperature to be 80-85 ℃, and controlling the running speed of the titanium belt to be 2.4-5.0 m/min.
And further, in the step eight, the alkali-washed liquid enters an air furnace gas heating furnace for drying, the furnace temperature is controlled below 200 ℃, and a drying process is generally carried out at 180 ℃.
Further, the standing and heat preservation time in the first step is 16-20 min.
And further, after the titanium strip coil is subjected to acid cleaning on the basis of the seventh step, the titanium strip coil enters a rolling mill for rolling, and after a finished product is rolled, the titanium strip coil is subjected to alkali cleaning with sodium hydroxide water solution to remove surface oil stains.
Further, after vacuumizing in the sixth step, continuously heating to 600-650 ℃, and preserving heat for 5-6 hours at a heating speed of 15-17 ℃/h.
Compared with the prior art, the invention has the beneficial effects that:
(1) the titanium strip coil processing technology enables the surface of a finished product to be smooth and clean, and the finished product is in a metal natural color. The annealed titanium strip coil can be supplied by acid pickling without sand blasting or polishing, only a small amount of finished product surface has slight darkening and local water marks, only a small amount of finished product has local defects of scratches, pressure marks, pits, spots, polishing marks and the like which are not more than half of the thickness tolerance, and the finished product surface has no macroscopic defects of cracks, peeling, oxide scale, pressing folds, metal and nonmetal inclusions and the like and marks after alkali and acid pickling.
(2) By applying the vacuum induction annealing method, the heating temperature of the titanium strip coil can be accurately controlled; the multi-station operation can respectively carry out heating and cooling, the equipment utilization rate is high, and the annealing efficiency is greatly improved. The heating mode is changed, the external heat is improved into self-heating, and the heating efficiency is greatly improved.
(3) Arc discharge is generated in the prepared electrolyte by utilizing the micro-arc oxidation technology, and a ceramic coating is obtained by in-situ growth on the surface of the cleaned and dried titanium strip coil metal, so that the ceramic coating effectively plays a role of preventing cracks, improves the overall strength of the titanium strip coil metal and has good heat resistance and corrosion resistance, thereby fundamentally overcoming the defects of aluminum, magnesium and titanium alloy materials in application, and therefore, the technology has wide application prospect.
(4) The titanium strip coil treatment process is stable and reliable, simple in equipment, convenient to operate, strong in practicability and suitable for wide popularization and use.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, 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.
Example 1
A titanium strip coil vacuum annealing treatment process comprises the following specific treatment process steps:
the method comprises the following steps: putting titanium ingots and leftover bits and pieces into a titanium melting furnace, converting the solid titanium ingots into liquid titanium water, and standing and preserving the temperature of the titanium water;
step two: allowing the titanium water after standing and heat preservation to flow into a casting and rolling machine through a pipeline, cooling by circulating water while flowing in, and continuously casting and rolling from the casting and rolling machine and then curling to obtain a titanium strip coil;
step three: removing oxide skin on the surface of the hot coil from the titanium strip coil obtained in the step two by adopting shot blasting and acid washing, and quickly drying by adopting an industrial hot air blower after cleaning;
step four: arc discharge is generated in the prepared electrolyte by utilizing the micro-arc oxidation technology on the basis of the third step, and a ceramic coating is obtained by in-situ growth on the metal surface of the cleaned and dried titanium strip coil;
step five: placing the titanium strip coil into an annealing furnace, purging the annealing furnace by using inert gas to completely replace the atmosphere in the annealing furnace, heating the titanium strip coil to 400-450 ℃ at a heating speed of 55-170 ℃/h, and preserving heat for 22-24 h;
step six: vacuumizing the annealing furnace to 10-4 Pa of vacuum degree; removing air, replacing the air with argon in the air removing process, and performing forced circulation through a fan to uniformly cool the air to 120-150 ℃ at a cooling speed of 5 ℃/h;
step seven: and (3) carrying out vacuum exhaust in the annealing furnace until the pressure is 3-5 multiplied by 10 < -2 > Pa, and then cooling to room temperature at the speed of 5-10 ℃/min to take out the titanium strip coil.
Wherein, the electrolyte prepared in the fourth step is one of Na2SO4, Na2CO3, Na2SiO3 and Na3PO4 which are commonly used.
In the third step, the steel shot granularity is 0.20-0.40 mm, the steel shot hardness is 50-55 HV, the projection speed is as follows: 55-70 m/s, projection density: 75-95 kg/m2, acid pickling for dephosphorization, using a mixed solution of 15-25% of nitric acid and 4-8% of hydrofluoric acid to carry out acid pickling for dephosphorization on the hot-rolled titanium coil, controlling the acid pickling temperature to be 80-85 ℃, and controlling the running speed of the titanium belt to be 2.4-5.0 m/min.
And in the eighth step, the alkali-washed mixture enters an air furnace and a gas heating furnace for drying, the furnace temperature is controlled below 200 ℃, and a drying process is generally carried out at 180 ℃.
Wherein, the standing and heat preservation time in the first step is 16-20 min.
The titanium strip is pickled and then rolled in a rolling mill, and after the rolled product is finished, the surface oil stain is removed by alkali washing of sodium hydroxide aqueous solution.
And sixthly, continuously heating to 600-650 ℃ after vacuumizing, and keeping the temperature for 5-6 h at a heating speed of 15-17 ℃/h.
Example 2
A titanium strip coil vacuum annealing treatment process comprises the following specific treatment process steps:
the method comprises the following steps: putting titanium ingots and leftover bits and pieces into a titanium melting furnace, converting the solid titanium ingots into liquid titanium water, and standing and preserving the temperature of the titanium water;
step two: allowing the titanium water after standing and heat preservation to flow into a casting and rolling machine through a pipeline, cooling by circulating water while flowing in, and continuously casting and rolling from the casting and rolling machine and then curling to obtain a titanium strip coil;
step three: removing oxide skin on the surface of the hot coil from the titanium strip coil obtained in the step two by adopting shot blasting and acid washing, and quickly drying by adopting an industrial hot air blower after cleaning;
step four: arc discharge is generated in the prepared electrolyte by utilizing the micro-arc oxidation technology on the basis of the third step, and a ceramic coating is obtained by in-situ growth on the metal surface of the cleaned and dried titanium strip coil;
step five: placing the titanium strip coil into an annealing furnace, purging the annealing furnace by using inert gas to completely replace the atmosphere in the annealing furnace, heating the titanium strip coil to 400-450 ℃ at a heating speed of 55-170 ℃/h, and preserving heat for 22-24 h;
step six: vacuumizing the annealing furnace to 10-4 Pa of vacuum degree; removing air, replacing the air with neon in the air removing process, and performing forced circulation through a fan to uniformly cool the air to 120-150 ℃ at a cooling speed of 5 ℃/h;
step seven: and (3) carrying out vacuum exhaust in the annealing furnace until the pressure is 3-5 multiplied by 10 < -2 > Pa, and then cooling to room temperature at the speed of 5-10 ℃/min to take out the titanium strip coil.
Wherein, the electrolyte prepared in the fourth step is one of Na2SO4, Na2CO3, Na2SiO3 and Na3PO4 which are commonly used.
In the third step, the steel shot granularity is 0.20-0.40 mm, the steel shot hardness is 50-55 HV, the projection speed is as follows: 55-70 m/s, projection density: 75-95 kg/m2, acid pickling for dephosphorization, using a mixed solution of 15-25% of nitric acid and 4-8% of hydrofluoric acid to carry out acid pickling for dephosphorization on the hot-rolled titanium coil, controlling the acid pickling temperature to be 80-85 ℃, and controlling the running speed of the titanium belt to be 2.4-5.0 m/min.
And in the eighth step, the alkali-washed mixture enters an air furnace and a gas heating furnace for drying, the furnace temperature is controlled below 200 ℃, and a drying process is generally carried out at 180 ℃.
Wherein, the standing and heat preservation time in the first step is 16-20 min.
The titanium strip is pickled and then rolled in a rolling mill, and after the rolled product is finished, the surface oil stain is removed by alkali washing of sodium hydroxide aqueous solution.
And sixthly, continuously heating to 600-650 ℃ after vacuumizing, and keeping the temperature for 5-6 h at a heating speed of 15-17 ℃/h.
When the invention works: the titanium strip coil processing technology enables the surface of a finished product to be smooth and clean, and the finished product is in a metal natural color. The annealed titanium strip coil can be supplied by acid pickling without sand blasting or polishing, slight darkening and local water marks exist on the surface of a small amount of finished products, only the small amount of finished products have defects of partial scratches, pressing marks, pits, spots, polishing marks and the like which are not more than half of the thickness tolerance, and the surface of the finished products have no macroscopic defects of cracks, peeling, oxide scale, pressing, metal and nonmetal inclusion and the like and marks after alkali and acid pickling; by applying the vacuum induction annealing method, the heating temperature of the titanium strip coil can be accurately controlled; the multi-station operation can respectively carry out heating and cooling, the equipment utilization rate is high, and the annealing efficiency is greatly improved. The heating mode is changed, the external heat is improved into self-heating, and the heating efficiency is greatly improved; arc discharge is generated in the prepared electrolyte by utilizing the micro-arc oxidation technology, and a ceramic coating is obtained by in-situ growth on the surface of the cleaned and dried titanium strip coil metal, so that the ceramic coating effectively plays a role of preventing cracks, improves the overall strength of the titanium strip coil metal and has good heat resistance and corrosion resistance, thereby fundamentally overcoming the defects of aluminum, magnesium and titanium alloy materials in application, and having wide application prospect; the titanium strip coil treatment process is stable and reliable, simple in equipment, convenient to operate, strong in practicability and suitable for wide popularization and use.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A titanium strip coil vacuum annealing treatment process is characterized by comprising the following specific treatment process steps:
the method comprises the following steps: putting titanium ingots and leftover bits and pieces into a titanium melting furnace, converting the solid titanium ingots into liquid titanium water, and standing and preserving the temperature of the titanium water;
step two: allowing the titanium water after standing and heat preservation to flow into a casting and rolling machine through a pipeline, cooling by circulating water while flowing in, and continuously casting and rolling from the casting and rolling machine and then curling to obtain a titanium strip coil;
step three: removing oxide skin on the surface of the hot coil from the titanium strip coil obtained in the step two by adopting shot blasting and acid washing, and quickly drying by adopting an industrial hot air blower after cleaning;
step four: arc discharge is generated in the prepared electrolyte by utilizing the micro-arc oxidation technology on the basis of the third step, and a ceramic coating is obtained by in-situ growth on the metal surface of the cleaned and dried titanium strip coil;
step five: placing the titanium strip coil into an annealing furnace, purging the annealing furnace by using inert gas to completely replace the atmosphere in the annealing furnace, heating the titanium strip coil to 400-450 ℃ at a heating speed of 55-170 ℃/h, and preserving heat for 22-24 h;
step six: vacuumizing the annealing furnace to 10-4 Pa of vacuum degree; removing air, replacing the air with argon in the air removing process, and performing forced circulation through a fan to uniformly cool the air to 120-150 ℃ at a cooling speed of 5 ℃/h;
step seven: and (3) carrying out vacuum exhaust in the annealing furnace until the pressure is 3-5 multiplied by 10 < -2 > Pa, and then cooling to room temperature at the speed of 5-10 ℃/min to take out the titanium strip coil.
2. The titanium strip coil vacuum annealing process according to claim 1, wherein: the electrolyte prepared in the fourth step is one of Na2SO4, Na2CO3, Na2SiO3 and Na3PO4 which are commonly used.
3. The titanium strip coil vacuum annealing process according to claim 1, wherein: in the third step, the steel shot granularity is 0.20-0.40 mm, the steel shot hardness is 50-55 HV, the projection speed is as follows: 55-70 m/s, projection density: 75-95 kg/m2, acid pickling for dephosphorization, using a mixed solution of 15-25% of nitric acid and 4-8% of hydrofluoric acid to carry out acid pickling for dephosphorization on the hot-rolled titanium coil, controlling the acid pickling temperature to be 80-85 ℃, and controlling the running speed of the titanium belt to be 2.4-5.0 m/min.
4. The titanium strip coil vacuum annealing process according to claim 1, wherein: and step eight, after alkali washing, drying the alkali-washed.
5. The titanium strip coil vacuum annealing process according to claim 1, wherein: the standing and heat preservation time in the first step is 16-20 min.
6. The titanium strip coil vacuum annealing process according to claim 1, wherein: and seventhly, pickling the titanium strip coil, then rolling the titanium strip coil in a rolling mill, and after rolling the finished product, performing alkaline washing on the sodium hydroxide water solution to remove surface oil stains.
7. The titanium strip coil vacuum annealing process according to claim 1, wherein: and in the sixth step, after vacuumizing, the heating is continued to 600-650 ℃, the temperature is kept for 5-6 h, and the heating speed is 15-17 ℃/h.
CN201911223122.6A 2019-12-03 2019-12-03 Vacuum annealing treatment process for titanium strip coil Pending CN110923597A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115821189A (en) * 2023-02-20 2023-03-21 湖南湘投金天钛金属股份有限公司 Heat treatment method of titanium strip coil for plate replacement

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323938A (en) * 2008-07-25 2008-12-17 武钢集团昆明钢铁股份有限公司 Process for cold rolling industry pure titanium coil annealing by cover-type annealing furnace
CN109137043A (en) * 2018-11-13 2019-01-04 西安庄信新材料科技有限公司 A kind of titanium or titanium alloy differential arc oxidation coating production technology

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323938A (en) * 2008-07-25 2008-12-17 武钢集团昆明钢铁股份有限公司 Process for cold rolling industry pure titanium coil annealing by cover-type annealing furnace
CN109137043A (en) * 2018-11-13 2019-01-04 西安庄信新材料科技有限公司 A kind of titanium or titanium alloy differential arc oxidation coating production technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115821189A (en) * 2023-02-20 2023-03-21 湖南湘投金天钛金属股份有限公司 Heat treatment method of titanium strip coil for plate replacement

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