CN114393055A - Preparation method of titanium strip coil for composite vacuum cup - Google Patents

Preparation method of titanium strip coil for composite vacuum cup Download PDF

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Publication number
CN114393055A
CN114393055A CN202111529811.7A CN202111529811A CN114393055A CN 114393055 A CN114393055 A CN 114393055A CN 202111529811 A CN202111529811 A CN 202111529811A CN 114393055 A CN114393055 A CN 114393055A
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titanium
strip coil
rolling
titanium strip
rolled
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肖瑛
任浩
张路路
高文柱
李建康
郭梦
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Xinjiang Xiangrun New Material Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/02Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1295Refining, melting, remelting, working up of titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04Refining by applying a vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • 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

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  • Engineering & Computer Science (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a preparation method of a titanium strip coil for a composite vacuum cup, which comprises the following steps: s1, smelting by using sponge titanium as a raw material to obtain a titanium ingot; s2, after turning and peeling the titanium cast ingot and locally grinding, heating and forging the titanium cast ingot into a slab, and then trimming the slab to obtain a finished slab; s3, carrying out hot rolling, acid pickling and annealing treatment on the refined plate blank to obtain a hot-rolled annealed titanium strip coil; s4, cold rolling the hot-rolled annealed titanium strip coil into a first-rolling-process titanium strip coil, and then carrying out acid pickling and annealing treatment on the first-rolling-process titanium strip coil to obtain an annealed titanium strip coil; s5, cold rolling the annealed titanium strip coil into a cold-rolled titanium strip coil; s6, degreasing and annealing the cold-rolled titanium strip coil to obtain a finished titanium strip coil; the invention has reasonable design and excellent mechanical property, and is suitable for large-scale popularization.

Description

Preparation method of titanium strip coil for composite vacuum cup
Technical Field
The invention relates to the technical field of titanium material processing, in particular to a preparation method of a titanium strip coil for a composite vacuum cup.
Background
The stainless steel vacuum heat-preservation vessel has the advantages of good heat-preservation performance, safety, portability, energy conservation, environmental protection, fashionable appearance, rich functions and the like. Scientific research shows that heavy metals can be separated out from stainless steel articles for daily use in the using process, so that great risk is brought to the health of users. Titanium metal is almost the only metal in the world which is completely harmless to human bodies, and is also a high-grade medical material which can be safely implanted into human bodies to become human organs. Therefore, titanium metal may be the best alternative to stainless steel.
Pure titanium household articles, as pets of a new era, are quietly brought into our lives, and are deeply welcomed by consumers because the pure titanium household articles have the characteristics of no dissolution of pathogenic carcinogenic heavy metals of nickel, chromium and manganese in high-temperature, acidic or alkaline food material environments, no rustiness, natural bacteriostasis, biological affinity, lasting freshness preservation, firmness, durability and the like.
However, in the prior art, because the content of impurity elements is difficult to control in the preparation process of the titanium strip coil, when the titanium strip coil is used for manufacturing the vacuum cup, the cup body is easy to wrinkle and crack, and the forming effect is poor.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of a titanium strip coil for a composite vacuum cup.
The technical scheme of the invention is as follows: a preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting titanium sponge with more than 1 grade as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, and performing assembly welding on the electrode block by using a plasma welding box and then performing twice smelting by using a vacuum consumable furnace to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe is less than or equal to 0.05 wt%, C is less than or equal to 0.02 wt%, N is less than or equal to 0.02 wt%, H is less than or equal to 0.010 wt%, O is less than or equal to 0.050 wt%, and the balance is Ti;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 25-35 mm by a four-high mill, and controlling the deformation of rough rolling to be 80-87%; then, finely rolling the titanium strips by a steckel mill to form a hot-rolled titanium strip coil with the thickness of 3.5-4.5 mm, and finally carrying out continuous pickling annealing treatment on the hot-rolled titanium strip coil, wherein the annealing temperature is controlled to be 700-750 ℃, and the stroke speed is 10-15 m/min, so as to obtain the hot-rolled annealed titanium strip coil;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-pass titanium strip coil with the thickness of 1.5-2.5 mm, then continuous acid pickling annealing treatment is carried out on the first-pass titanium strip coil, the annealing temperature is controlled to be 600-700 ℃, and the stroke speed is 10-15 m/min, so that the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 50-55%, and the rolling deformation of each pass is controlled to be 5-10%;
s5, second rolling process
Cold-rolling the annealed titanium strip coil obtained in the step S4 into a cold-rolled titanium strip coil with the thickness of 0.35-0.45 mm in multiple passes; in the second rolling process, the total rolling deformation is controlled to be 80-85%, and the rolling deformation of each pass is controlled to be 5-10%;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 10-20 m/min, performing bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is completed, controlling the annealing temperature to be 620-640 ℃, performing heat preservation treatment for 10-15 h, and naturally cooling the materials to obtain a finished product of the titanium strip coil.
Further, in the step S6, degreasing the cold-rolled titanium strip coil in an electrolytic degreasing mode, wherein the temperature is controlled to be 65-85 ℃ in the degreasing process; the electrolytic degreasing mode is favorable for reducing the degreasing solution residue on the surface of the cold-rolled titanium strip coil and improving the degreasing effect of the cold-rolled titanium strip coil.
Further, in step S1, the electrode block is assembled by using a vacuum plasma welding box, and arc stabilization is well controlled during welding without arc interruption; the oxidation in the welding process of the electrode block can be avoided, and meanwhile, the welding quality can be improved.
Further, in step S1, the two times of melting of the electrode block after the assembly welding specifically include: firstly, placing the assembled and welded electrode block into a vacuum consumable electrode furnace for primary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.02-0.05 Pa, the smelting temperature to be 1600-1800 ℃ and the smelting time to be 1-2 h, and carrying out primary water cooling on a titanium metal solution after smelting is finished to form a semi-finished product titanium ingot; wherein, the water pressure of the primary water-cooling circulation is controlled to be 0.5-0.8 MPa; then placing the semi-finished product titanium ingot into a vacuum consumable electrode furnace for secondary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.06-0.1 Pa, the smelting temperature to be 1900-2000 ℃, and the smelting time to be 2-3 h, and carrying out secondary water cooling on a titanium metal solution after smelting is finished to form a titanium ingot; wherein the water pressure of the secondary water-cooling circulation is controlled to be 0.3-0.5 MPa; the electrode block after the assembly welding is smelted under different smelting conditions, so that the segregation degree of dendritic crystals in the titanium ingot can be reduced, and meanwhile, the mechanical property of the titanium ingot can be improved.
Further, in step S3, the work rolls of the four-high rolling mill are made of heat-resistant die steel, the roughness of the roll surfaces of the rolls is less than or equal to 0.01 μm, and the surface smoothness and mechanical properties of the hot-rolled annealed titanium strip coil can be ensured by controlling the roughness of the roll surfaces of the rolls.
Further, in step S1, in the process of smelting the electrode block after the assembly welding, introducing the titanium metal solution into a degassing device for degassing treatment, and controlling the hydrogen content in the degassing device to be less than 0.12mL/100g ti; then filtering the weathered titanium metal solution; by degassing and filtering the titanium metal solution, the defects of slag inclusion, looseness and the like of the titanium cast ingot can be avoided, and the stress concentration phenomenon of the titanium cast ingot is avoided.
Further, in step S2, the titanium ingot forging is specifically operated as: firstly, placing a titanium ingot in a box-type resistance furnace, heating to 900-1050 ℃, then carrying out upsetting and drawing forging on the titanium ingot by using a 1800-2400T quick forging machine, carrying out regression forging at 950-1000 ℃ in the middle, and repeating upsetting and drawing forging for three times to obtain a plate blank; by forging the titanium ingot for multiple times, the refinement degree of the grain size in the titanium ingot can be promoted, so that the uniformity of the internal structure of the titanium ingot is promoted.
Further, before the step S1, drying the titanium sponge raw material for 2-5 hours under the conditions that the vacuum degree is 3-6 Pa and the temperature is 110-160 ℃; moisture in the titanium sponge raw material is removed through drying treatment, and the generation of impurity gas in the smelting process of the titanium sponge raw material is avoided.
Further, in step S5, reversing the annealed titanium strip coil in each pass of rolling; by reversing rolling the annealed titanium strip coil, the groove-shaped defect caused by uneven deformation on the surface of the finished titanium strip coil can be avoided.
Further, in step S6, when the titanium strip coil is subjected to degreasing treatment, the degreasing agent is prepared by compounding potassium pyrophosphate, sodium tripolyphosphate, alkylphenol ethoxylates, benzotriazole and purified water according to a volume ratio of 2:3:2:1: 5; the degreasing agent has strong degreasing capability and does not corrode the surface of the cold-rolled titanium strip coil.
Compared with the prior art, the beneficial effects of the invention are embodied in the following points:
firstly, the invention uses sponge titanium with more than 1 grade as raw material, scientifically controls the content of each impurity element in the raw material, adjusts the production process measures of the product and realizes the matching of each performance of the product; the defects of surface wrinkling, uneven deformation after bulging and surface cracking when the titanium strip for the composite vacuum cup is coiled and welded into a pipe are overcome;
secondly, the invention can make the mechanical property, the process property and the grain size of the finished product of the titanium strip coil well matched by researching the continuous annealing process of the titanium strip coil for the composite vacuum cup; thereby improving the stability of the mechanical property of the titanium strip coil finished product;
thirdly, the cold rolling process of the titanium strip coil is divided into a first rolling process and a second rolling process, so that the surface flatness and the thickness uniformity of the titanium strip coil can be improved, the grain size refinement degree and the structure uniformity of the titanium strip coil can be promoted, and the metal performance of a finished titanium strip coil is improved.
Detailed Description
Example 1
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, and performing assembly welding on the electrode block by using a vacuum plasma welding box and then performing twice smelting by using a vacuum consumable furnace to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.05 wt%, C is less than or equal to: 0.02 wt%, N: 0.02 wt%, H: 0.010 wt%, O: 0.050 wt% and the balance Ti;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 25mm by a four-high mill, and controlling the deformation of rough rolling to be 80%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 3.5mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 700 ℃, and the stroke speed is 10m/min, so that hot-rolled and annealed titanium strip coils are obtained;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 1.5mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 600 ℃, and the stroke speed is 10m/min, so that the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 50%, and the rolling deformation of each pass is controlled to be 5%;
s5, second rolling process
Carrying out multi-pass cold rolling on the annealed titanium strip coil obtained in the step S4 to obtain a cold-rolled titanium strip coil with the thickness of 0.35 mm; in the second rolling process, the total rolling deformation is controlled to be 80%, and the rolling deformation of each pass is controlled to be 5%;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 10m/min, carrying out bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is finished, controlling the annealing temperature to be 620 ℃, carrying out heat preservation treatment for 10h, and naturally cooling the material to obtain a finished product of the titanium strip coil.
Example 2
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, and performing assembly welding on the electrode block by using a vacuum plasma welding box and then performing twice smelting by using a vacuum consumable furnace to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.04 wt%, C: 0.01 wt%, N: 0.01 wt%, H: 0.008 wt%, O: 0.045 wt%, the balance being Ti;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 32mm by a four-high mill, and controlling the deformation of rough rolling to be 83%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 3.8mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 730 ℃, and the stroke speed is 12m/min, so that hot-rolled and annealed titanium strip coils are obtained; wherein, the working roll of the four-high mill is made of heat-resistant die steel, and the roughness of the roll surface of the roll is 0.01 μm. The surface smoothness and the mechanical property of the hot-rolled annealed titanium strip coil can be ensured by controlling the roughness of the roll surface of the roll;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 2.2mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 680 ℃, the stroke speed is 12m/min, and the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 52 percent, and the rolling deformation of each pass is controlled to be 8 percent;
s5, second rolling process
Carrying out multi-pass cold rolling on the annealed titanium strip coil obtained in the step S4 to obtain a cold-rolled titanium strip coil with the thickness of 0.42 mm; in the second rolling process, the total rolling deformation is controlled to be 83 percent, and the rolling deformation of each pass is controlled to be 9 percent;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 16m/min, carrying out bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is finished, controlling the annealing temperature to be 630 ℃, carrying out heat preservation treatment for 12h, and naturally cooling the materials to obtain a finished product of the titanium strip coil.
Example 3
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, and then drying the titanium sponge raw material for 2 hours under the conditions that the vacuum degree is 3Pa and the temperature is 110 ℃; removing water in the titanium sponge raw material through drying treatment, avoiding the generation of impurity gas in the smelting process of the titanium sponge raw material, pressing the dried titanium sponge into an electrode block, and then performing two-time smelting on the electrode block through a vacuum consumable electrode furnace after the electrode block is subjected to assembly welding through a vacuum plasma welding box to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.05 wt%, C: 0.02 wt%, N: 0.02 wt%, H: 0.010 wt%, O: 0.050 wt% and the balance Ti; the two-time smelting specifically comprises the following steps: firstly, placing the electrode block after assembly welding into a vacuum consumable electrode furnace for primary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.02Pa, the smelting temperature to be 1600 ℃, and the smelting time to be 1h, and carrying out primary water cooling on a titanium metal solution after smelting is finished to form a semi-finished product titanium ingot; wherein, the water pressure of the primary water cooling circulation is controlled to be 0.5 MPa; then placing the semi-finished product titanium ingot into a vacuum consumable electrode furnace for secondary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.06Pa, the smelting temperature to be 1900 ℃, and the smelting time to be 2 hours, and carrying out secondary water cooling on a titanium metal solution after smelting is finished to form a titanium ingot; wherein, the water pressure of the secondary water-cooling circulation is controlled to be 0.3 MPa; the electrode block after the assembly welding is smelted under different smelting conditions, so that the segregation degree of dendritic crystals in the titanium ingot can be reduced, and the mechanical property of the titanium ingot can be improved;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 35mm by a four-high mill, and controlling the deformation of rough rolling to be 87%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 4.5mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 750 ℃, and the stroke speed is 15m/min, so as to obtain hot-rolled and annealed titanium strip coils;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 2.5mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 700 ℃, the stroke speed is 15m/min, and the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 55%, and the rolling deformation of each pass is controlled to be 10%;
s5, second rolling process
The annealed titanium strip coil obtained in the step S4 is subjected to multi-pass cold rolling to form a cold-rolled titanium strip coil with the thickness of 0.45 mm; in the second rolling process, the total rolling deformation is controlled to be 85 percent, and the rolling deformation of each pass is controlled to be 10 percent;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 20m/min, performing bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is finished, controlling the annealing temperature to be 640 ℃, performing heat preservation treatment for 15h, and naturally cooling the material to obtain a finished product of the titanium strip coil.
Example 4
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, and performing assembly welding on the electrode block by using a vacuum plasma welding box and then performing twice smelting by using a vacuum consumable furnace to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.05 wt%, C: 0.02 wt%, N: 0.02 wt%, H: 0.010 wt%, O: 0.050 wt% and the balance Ti; in the smelting process of the electrode block after the assembly welding, introducing a titanium metal solution into a degassing device for degassing treatment, and controlling the hydrogen content in the degassing device to be 0.11mL/100 gTi; then filtering the weathered titanium metal solution; by degassing and filtering the titanium metal solution, the defects of slag inclusion, looseness and the like of the titanium cast ingot can be avoided, so that the stress concentration phenomenon of the titanium cast ingot is avoided;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 25mm by a four-high mill, and controlling the deformation of rough rolling to be 80%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 3.5mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 700 ℃, and the stroke speed is 10m/min, so that hot-rolled and annealed titanium strip coils are obtained;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 1.5mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 600 ℃, and the stroke speed is 10m/min, so that the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 50%, and the rolling deformation of each pass is controlled to be 5%;
s5, second rolling process
The annealed titanium strip coil obtained in the step S4 is subjected to multi-pass cold rolling to form a cold-rolled titanium strip coil with the thickness of 0.45 mm; in the second rolling process, the total rolling deformation is controlled to be 85 percent, and the rolling deformation of each pass is controlled to be 7 percent;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 16m/min, carrying out bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is finished, controlling the annealing temperature to be 630 ℃, carrying out heat preservation treatment for 12h, and naturally cooling the materials to obtain a finished product of the titanium strip coil.
Example 5
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, and performing assembly welding on the electrode block by using a vacuum plasma welding box and then performing twice smelting by using a vacuum consumable furnace to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.05 wt%, C: 0.02 wt%, N: 0.02 wt%, H: 0.010 wt%, O: 0.050 wt% and the balance Ti;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab; the titanium ingot casting forging operation is as follows: firstly, placing a titanium cast ingot in a box-type resistance furnace, heating to 900 ℃, then carrying out upsetting and stretching forging on the titanium cast ingot by using a 1800T quick forging machine, carrying out regressing forging at the middle temperature of 950 ℃, and repeatedly upsetting and stretching forging for three times to obtain a first plate blank; the refining degree of the grain size in the titanium cast ingot can be promoted by forging the titanium cast ingot for multiple times, so that the uniformity of the internal structure of the titanium cast ingot is promoted;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 35mm by a four-high mill, and controlling the deformation of rough rolling to be 87%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 4.5mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 750 ℃, and the stroke speed is 15m/min, so as to obtain hot-rolled and annealed titanium strip coils;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 2.5mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 700 ℃, the stroke speed is 15m/min, and the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 55%, and the rolling deformation of each pass is controlled to be 10%;
s5, second rolling process
The annealed titanium strip coil obtained in the step S4 is subjected to multi-pass cold rolling to form a cold-rolled titanium strip coil with the thickness of 0.45 mm; in the second rolling process, the total rolling deformation is controlled to be 85 percent, and the rolling deformation of each pass is controlled to be 10 percent;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 20m/min, performing bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is finished, controlling the annealing temperature to be 640 ℃, performing heat preservation treatment for 15h, and naturally cooling the material to obtain a finished product of the titanium strip coil.
Example 6
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, and performing assembly welding on the electrode block by using an equal vacuum plasma welding box and then performing twice smelting by using a vacuum consumable furnace to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.05 wt%, C: 0.02 wt%, N: 0.02 wt%, H: 0.010 wt%, O: 0.050 wt% and the balance Ti;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 25mm by a four-high mill, and controlling the deformation of rough rolling to be 85%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 4.2mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled at 735 ℃ and the stroke speed is 12m/min, so as to obtain hot-rolled and annealed titanium strip coils;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 2.2mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 680 ℃, the stroke speed is 12m/min, and the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 53 percent, and the rolling deformation of each pass is controlled to be 9 percent;
s5, second rolling process
The annealed titanium strip coil obtained in the step S4 is subjected to multi-pass cold rolling to form a cold-rolled titanium strip coil with the thickness of 0.45 mm; in the second rolling process, the total rolling deformation is controlled to be 85 percent, and the rolling deformation of each pass is controlled to be 5 percent; in each rolling process, reversing rolling is carried out on the annealed titanium strip coil; by reversing rolling the annealed titanium strip coil, the groove-shaped defect caused by uneven deformation on the surface of a finished titanium strip coil product can be avoided;
s6, degreasing and annealing
Performing electrolytic degreasing treatment on the cold-rolled titanium strip coil obtained in the step S5, controlling the degreasing speed to be 13m/min and the degreasing temperature to be 85 ℃, performing bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is completed, controlling the annealing temperature to be 620 ℃, performing heat preservation treatment for 10 hours, and naturally cooling the materials to obtain a finished product of the titanium strip coil; when the cold-rolled titanium strip coil is degreased, the degreasing agent is prepared by compounding potassium pyrophosphate, sodium tripolyphosphate, alkylphenol polyoxyethylene, benzotriazole and purified water according to the volume ratio of 2:3:2:1: 5.
Example 7
A preparation method of a titanium strip coil for a composite vacuum cup comprises the following steps:
s1, selecting and smelting
Selecting 0-grade titanium sponge as a raw material, stirring the titanium sponge raw material by using a mixer, and then drying the titanium sponge raw material for 5 hours under the conditions that the vacuum degree is 6Pa and the temperature is 160 ℃; removing water in the titanium sponge raw material through drying treatment, avoiding the generation of impurity gas in the smelting process of the titanium sponge raw material, pressing the dried titanium sponge raw material into an electrode block, and finally performing two-time smelting on the electrode block through a vacuum consumable furnace after the electrode block is subjected to assembly welding in a plasma welding box to obtain a titanium ingot; the mass percentage of each element in the titanium ingot is as follows: fe: 0.05 wt%, C: 0.02 wt%, N: 0.02 wt%, H: 0.010 wt%, O: 0.050 wt% and the balance Ti; the two-time smelting specifically comprises the following steps: firstly, placing the electrode block after assembly welding into a vacuum consumable electrode furnace for primary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.05Pa, the smelting temperature to be 1800 ℃ and the smelting time to be 2 hours, and carrying out primary water cooling on a titanium metal solution after smelting is finished to form a semi-finished product titanium ingot; wherein, the water pressure of the primary water cooling circulation is controlled to be 0.8 MPa; then placing the semi-finished product titanium ingot into a vacuum consumable electrode furnace for secondary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.1Pa, the smelting temperature to be 2000 ℃, and the smelting time to be 3 hours, and carrying out secondary water cooling on a titanium metal solution after the smelting is finished to form a titanium ingot; wherein, the water pressure of the secondary water-cooling circulation is controlled to be 0.5 MPa; the electrode block after the assembly welding is smelted under different smelting conditions, so that the segregation degree of dendritic crystals in the titanium ingot can be reduced, and the mechanical property of the titanium ingot can be improved; in the smelting process of the electrode block after the assembly welding, introducing a titanium metal solution into a degassing device for degassing treatment, and controlling the hydrogen content in the degassing device to be 0.08mL/100 gTi; then filtering the weathered titanium metal solution; by degassing and filtering the titanium metal solution, the defects of slag inclusion, looseness and the like of the titanium cast ingot can be avoided, so that the stress concentration phenomenon of the titanium cast ingot is avoided;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a slab, then planing and milling the upper surface, the lower surface and two side surfaces of the slab, and finally chamfering edges and corners in the length direction of the slab to obtain a refined slab; the titanium ingot casting forging operation is as follows: firstly, placing a titanium cast ingot in a box-type resistance furnace, heating to 1050 ℃, then carrying out upsetting and drawing forging on the titanium cast ingot by using a 2400T quick forging machine, carrying out regressive forging on the titanium cast ingot at 1000 ℃, and repeatedly upsetting, drawing and forging for three times to obtain a plate blank; the refining degree of the grain size in the titanium cast ingot can be promoted by forging the titanium cast ingot for multiple times, so that the uniformity of the internal structure of the titanium cast ingot is promoted;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 35mm by a four-high mill, and controlling the deformation of rough rolling to be 87%; then, finely rolling the titanium strips into hot-rolled titanium strip coils with the thickness of 4.5mm by using a steckel mill, and finally carrying out continuous acid pickling and annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 750 ℃, and the stroke speed is 15m/min, so as to obtain hot-rolled and annealed titanium strip coils; wherein the working roll of the four-high mill is made of heat-resistant die steel, the surface roughness of the roll is 0.01 mu m, and the surface smoothness and the mechanical property of the hot-rolled annealed titanium strip coil can be ensured by controlling the surface roughness of the roll;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-rolling titanium strip coil with the thickness of 1.5mm, then the first-rolling titanium strip coil is subjected to continuous acid-washing annealing treatment, the annealing temperature is controlled to be 700 ℃, and the stroke speed is 10m/min, so that the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 50%, and the rolling deformation of each pass is controlled to be 7%;
s5, second rolling process
Carrying out multi-pass cold rolling on the annealed titanium strip coil obtained in the step S4 to obtain a cold-rolled titanium strip coil with the thickness of 0.35 mm; in the second rolling process, the total rolling deformation is controlled to be 80%, and the rolling deformation of each pass is controlled to be 7%; in each rolling process, reversing rolling is carried out on the annealed titanium strip coil; by reversing rolling the annealed titanium strip coil, the groove-shaped defect caused by uneven deformation on the surface of a finished titanium strip coil product can be avoided;
s6, degreasing and annealing
Performing electrolytic degreasing treatment on the cold-rolled titanium strip coil obtained in the step S5, controlling the degreasing speed to be 10m/min and the degreasing temperature to be 65 ℃, performing bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is completed, controlling the annealing temperature to be 630 ℃, and performing heat preservation treatment for 13h, and obtaining a finished product of the titanium strip coil after the materials are naturally cooled; when the cold-rolled titanium strip coil is degreased, the degreasing agent is prepared by compounding potassium pyrophosphate, sodium tripolyphosphate, alkylphenol polyoxyethylene, benzotriazole and purified water according to the volume ratio of 2:3:2:1: 5.
Test examples
The performance of the titanium strip coil finished products prepared in the embodiments 1 to 7 of the invention was tested, and the test results are shown in table 1:
TABLE 1 Effect of the examples on the Properties of a rolled titanium strip
Figure BDA0003410366270000151
As can be seen from the data in Table 1, in example 2, compared with example 1, the surface smoothness and the mechanical properties of the hot-rolled annealed titanium strip coil can be ensured by controlling the quality and the surface roughness of the working rolls of the four-high rolling mill; compared with the embodiment 1, the embodiment 3 has the advantages that the segregation degree of dendrites in the titanium ingot can be reduced and the mechanical property of the titanium ingot can be improved completely by smelting the electrode block subjected to the butt welding under different smelting conditions; moisture in the titanium sponge raw material is removed through drying treatment, so that the generation of impurity gas in the smelting process of the titanium sponge raw material is avoided; example 4 compared to example 1, by forging a titanium ingot multiple times, the degree of refinement of the grain size in the titanium ingot can be promoted, and the uniformity of the internal structure of the titanium ingot can be promoted; example 5 compared with example 1, by forging a titanium ingot a plurality of times, the degree of refinement of the grain size in the titanium ingot can be promoted, and the uniformity of the internal structure of the titanium ingot can be promoted; compared with the embodiment 1, the embodiment 6 can avoid the groove-shaped defects caused by uneven deformation on the surface of the finished titanium strip coil by reversing and rolling the annealed titanium strip coil; the degreasing agent has strong degreasing capability and does not corrode the surface of the cold-rolled titanium strip coil; compared with the embodiments 1 to 6, in the preparation process of the titanium strip coil finished product, the content of each element in the raw material is scientifically controlled, and the process parameters are optimally designed, so that each performance of the titanium strip coil finished product reaches the optimal use state.

Claims (10)

1. A preparation method of a titanium strip coil for a composite vacuum cup is characterized by comprising the following steps:
s1, selecting and smelting
Selecting titanium sponge with more than 1 grade as a raw material, stirring the titanium sponge raw material by using a mixer, pressing the titanium sponge raw material into an electrode block, welding the electrode block, and then smelting the electrode block twice by using a vacuum consumable electrode furnace to obtain a titanium ingot; the mass percentage composition of each element in the titanium ingot is as follows: fe is less than or equal to 0.05 wt%, C is less than or equal to 0.02 wt%, N is less than or equal to 0.02 wt%, H is less than or equal to 0.010 wt%, O is less than or equal to 0.050 wt%, and the balance is Ti;
s2 forging
Turning and peeling the titanium cast ingot obtained in the step S1, locally grinding, heating and forging to form a plate blank, then carrying out planing and milling treatment on the upper surface, the lower surface and two side surfaces of the plate blank, and finally carrying out chamfering treatment on edges and corners in the length direction of the plate blank to obtain a refined plate blank;
s3, hot rolling
Roughly rolling the refined plate blank obtained in the step S2 into a titanium strip coil with the thickness of 25-35 mm by a four-high mill, and controlling the deformation of rough rolling to be 80-87%; then, finely rolling the titanium strips by a steckel mill to form hot-rolled titanium strip coils with the thickness of 3.5-4.5 mm, and finally carrying out continuous pickling annealing treatment on the hot-rolled titanium strip coils, wherein the annealing temperature is controlled to be 700-750 ℃, the stroke speed is 10-15 m/min, so that hot-rolled annealed titanium strip coils are obtained;
s4, first rolling process
The hot-rolled annealed titanium strip coil obtained in the step S3 is subjected to multi-pass cold rolling to form a first-pass titanium strip coil with the thickness of 1.5-2.5 mm, then continuous acid pickling annealing treatment is carried out on the first-pass titanium strip coil, the annealing temperature is controlled to be 600-700 ℃, and the stroke speed is 10-15 m/min, so that the annealed titanium strip coil is obtained; in the first rolling process, the total rolling deformation is controlled to be 50-55%, and the rolling deformation of each pass is controlled to be 5-10%;
s5, second rolling process
Cold-rolling the annealed titanium strip coil obtained in the step S4 into a cold-rolled titanium strip coil with the thickness of 0.35-0.45 mm in multiple passes; in the second rolling process, the total rolling deformation is controlled to be 80-85%, and the rolling deformation of each pass is controlled to be 5-10%;
s6, degreasing and annealing
And (5) degreasing the cold-rolled titanium strip coil obtained in the step (S5), controlling the degreasing speed to be 10-20 m/min, performing bell-type furnace annealing on the cold-rolled titanium strip coil after degreasing is completed, controlling the annealing temperature to be 620-640 ℃, performing heat preservation treatment for 10-15 h, and naturally cooling the materials to obtain a finished product of the titanium strip coil.
2. The method for preparing the titanium strip coil for the composite vacuum cup as claimed in claim 1, wherein in the step S6, the cold-rolled titanium strip coil is degreased in an electrolytic degreasing manner, and the temperature is controlled to be 65-85 ℃ in the degreasing process.
3. The method for preparing a titanium tape roll for a composite vacuum cup as claimed in claim 1, wherein in step S1, said electrode block is assembled by using a vacuum plasma welding box.
4. The method for preparing the titanium strip for the composite vacuum cup according to claim 1, wherein in the step S1, the two times of smelting of the electrode block after the assembly welding specifically comprises: firstly, placing the assembled and welded electrode block into a vacuum consumable electrode furnace for primary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.02-0.05 Pa, the smelting temperature to be 1600-1800 ℃ and the smelting time to be 1-2 h, and carrying out primary water cooling on a titanium metal solution after smelting is finished to form a semi-finished product titanium ingot; wherein, the water pressure of the primary water-cooling circulation is controlled to be 0.5-0.8 MPa; then placing the semi-finished product titanium ingot into a vacuum consumable electrode furnace for secondary smelting, controlling the vacuum degree of the vacuum consumable electrode furnace to be 0.06-0.1 Pa, the smelting temperature to be 1900-2000 ℃, and the smelting time to be 2-3 h, and performing secondary water cooling on a titanium metal solution after smelting is finished to form a titanium ingot; wherein the water pressure of the secondary water-cooling circulation is controlled to be 0.3-0.5 MPa.
5. The method for preparing a titanium strip for a composite heat preservation cup according to claim 1, wherein in step S3, the work roll of the four-high mill is made of heat-resistant die steel, and the roughness of the roll surface of the roll is less than or equal to 0.01 μm.
6. The method for preparing the titanium strip for the composite vacuum cup as claimed in claim 1, wherein in step S1, in the process of smelting the assembled and welded electrode block, a titanium metal solution is introduced into a degassing device for degassing treatment, and the hydrogen content in the degassing device is controlled to be less than 0.12mL/100g of al; the weathered titanium metal solution is then filtered.
7. The method for preparing a titanium strip for a composite vacuum cup as claimed in claim 1, wherein in step S2, the titanium ingot forging operation is: firstly, placing a titanium ingot in a box-type resistance furnace, heating to 900-1050 ℃, then carrying out upsetting and drawing forging on the titanium ingot by using a 1800-2400T quick forging machine, carrying out regression forging on the titanium ingot at 950-1000 ℃, and repeating upsetting and drawing forging for three times to obtain a plate blank.
8. The method for preparing the titanium strip for the composite vacuum cup as claimed in claim 1, wherein before the step S1, the titanium sponge raw material is dried for 2-5 hours under the conditions of a vacuum degree of 3-6 Pa and a temperature of 110-160 ℃.
9. The method for preparing a titanium strip for a composite heat preservation cup according to claim 1, wherein in the step S5, the annealed titanium strip coil is reversely rolled in each rolling process.
10. The method of claim 1, wherein in step S1, the work rolls of the four-high rolling mill are made of die steel.
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