A titanium base material production method capable of shortening a titanium electrode production process
By omitting the sandblasting and thermal straightening processes and adopting a titanium palladium acid etching method for preparing metal composite plates, the problems of low production efficiency and easy oxidation of the substrate for titanium electrodes are solved, achieving efficient and low-cost titanium electrode preparation and improving the durability of the electrodes and the uniformity of the substrate.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- XIAN TAIJIN NEW ENERGY & MATERIALS SCI TECH CO LTD
- Filing Date
- 2023-03-09
- Publication Date
- 2026-07-03
AI Technical Summary
Existing titanium electrode manufacturing processes are complex and inefficient. The titanium substrate is easily oxidized, leading to electrode failure. Sandblasting and thermal straightening processes affect the uniformity and structure of the substrate, resulting in performance degradation.
By omitting the sandblasting and hot straightening processes, a titanium-palladium acid-etched metal composite plate preparation method is adopted. The plate is prepared by assembling a titanium plate and a titanium-palladium acid-etched metal alloy plate, followed by rolling, annealing and acid etching treatment, thus producing a porous titanium-based titanium-palladium metal composite plate, which improves oxidation resistance and roughness uniformity.
It shortens the titanium electrode production cycle, reduces costs, improves production efficiency and electrode durability, and ensures the uniformity of the substrate structure and the electrode life.
Smart Images
Figure CN116445696B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of electrode material preparation technology, and specifically to a method for preparing a titanium substrate that can shorten the preparation process of a titanium electrode. Background Technology
[0002] Titanium-coated electrodes, also known as metal anodes, are generally referred to domestically and internationally as DSA (Dimensionally Stable Anode). Developed in the late 1960s, they are a new type of high-efficiency electrode material. Titanium serves as the substrate because it is a valve-type metal; it conducts electricity in brine as a cathode but immediately becomes non-conductive as an anode. By coating it with an enamel-electrocatalytic-semiconductor coating, it becomes a corrosion-resistant anode with excellent conductivity. The greatest advantages of titanium as an electrode substrate material are its excellent chemical durability and machinability. Titanium-based active coated electrodes are an important type of electrolytic electrode. In recent years, with rapid market development, the market demands increasingly higher quality titanium-based active coated electrodes. These demands include not only good durability and high catalytic activity but also customized products with diverse dimensions and appearances, while maintaining strict control over production cycles and prices.
[0003] However, the manufacturing process of titanium electrodes is extremely complex, involving various steps such as material cutting, sandblasting, thermal straightening, acid etching, and coating. This results in a lengthy processing time and extremely low production efficiency. Furthermore, the sandblasting and thermal straightening processes cause significant damage to the microstructure and structure of the titanium substrate, leading to substantial performance degradation of the titanium electrode. Mechanical sandblasting cannot guarantee the uniformity of the roughness of the sandblasted titanium substrate, and the high sandblasting pressure worsens the flatness of the titanium substrate, requiring high-temperature thermal straightening to obtain a flat titanium substrate. However, high-temperature thermal straightening significantly alters the microstructure of the titanium substrate, affecting the lifespan of the titanium electrode. At the same time, the failure mode of electrodes prepared by traditional methods is generally as follows: during the electrolysis process, the active oxygen generated by the oxygen evolution reaction diffuses to the surface of the titanium substrate, oxidizing the titanium substrate and forming a TiO2 passivation layer, leading to the failure of the titanium electrode.
[0004] Therefore, the existing production process has the following defects: 1. The production process of titanium electrodes has a long cycle, low production efficiency, and high production cost; 2. The titanium substrate of titanium electrodes is easily oxidized, which will lead to the failure of titanium electrodes; 3. In the traditional process, the sandblasting process cannot guarantee the uniformity of the roughness of the titanium substrate; 4. In the traditional process, the heat straightening process will change the microstructure of the titanium substrate, affecting the performance and life of the titanium electrode. Summary of the Invention
[0005] This invention provides a method for preparing titanium substrate that can shorten the titanium electrode preparation process. It omits the sandblasting and shaping steps in the titanium electrode preparation process, thereby shortening the titanium electrode production process, improving production efficiency, and reducing production costs. The addition of the precious metal palladium enhances the oxidation resistance of the titanium substrate, thereby improving the durability of the titanium electrode. It can ensure that the titanium substrate used to prepare the titanium electrode has uniform roughness, avoid changes in the microstructure of the titanium substrate, and improve the lifespan and product performance of the titanium electrode.
[0006] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing a titanium substrate that can shorten the titanium electrode preparation process, comprising the following steps:
[0007] Step 1: Titanium plate preparation;
[0008] Step 2: Preparation of Titanium Palladium Acid-Corroded Metal Alloy Plate: Titanium powder, palladium powder, and acid-corroded metal powder are mixed, pressed, and welded into electrodes. The electrodes are melted into ingots, and the ingots are forged and shaped into titanium palladium acid-corroded metal composite blanks. The titanium palladium acid-corroded metal composite blanks are rolled and annealed to obtain hot-rolled coils with a grain size of 8-10 and uniform grain size. The hot-rolled coils are then rolled and annealed to become titanium palladium acid-corroded metal alloy plates, wherein the palladium content is 0.06%-0.08%, and the acid-corroded metal content is 1.00%-15.20%. The acid-corroded metal is a metal that can be corroded by acid.
[0009] Step 3: Preparation of titanium-based titanium-palladium metal composite plate: The titanium plate prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate prepared in Step 2 are assembled into a blank, with at least one side of the titanium plate being composited with the titanium-palladium acid-etched metal alloy plate. Then, the surface oxide scale is removed by annealing. Finally, the formed composite plate is immersed in an acid solution until the acid-etched metal is completely dissolved to obtain a porous titanium-based titanium-palladium metal composite plate.
[0010] Preferably, the titanium plate preparation in step one is as follows: pressing and welding titanium powder into electrodes, melting the electrodes into ingots, forging and shaping the ingots into titanium plate blanks with fragmented and uniform as-cast structure, rolling and annealing the titanium plate blanks to obtain hot-rolled coils with a grain size of 6-10 and uniform grain size, and then rolling and annealing the hot-rolled coils to obtain titanium plates.
[0011] Preferably, the thickness of the titanium slab in step one is 120-200 mm.
[0012] Preferably, in step one, the titanium slab is rolled into a coil with a thickness of 3mm to 5mm, and after annealing at 650℃ to 750℃, the oxide scale is removed to obtain a hot-rolled coil.
[0013] Preferably, in step one, the hot-rolled coil is rolled in multiple passes, with a pass deformation of ≤12%, a rolling stroke deformation of 30% to 55%, and a rolling speed of 50 to 180 m / min; then it is annealed at a temperature of 620 to 720°C for a holding time of 0.5 to 10 h.
[0014] Preferably, the thickness of the titanium palladium acid-etched metal composite slab obtained in step two is 20–80 mm.
[0015] Preferably, in step two, the titanium palladium acid-etched metal composite slab is rolled into a coil with a thickness of 0.5 mm to 1 mm, and after annealing at 650°C to 750°C, the surface oxide scale is removed to obtain a hot-rolled coil.
[0016] Preferably, in step two, the hot-rolled coil is rolled in multiple passes, with a deformation per pass ≤12%, a deformation per rolling pass of 30% to 55%, and a rolling speed of 50 to 180 m / min; then it is annealed at a temperature of 620 to 720°C for a holding time of 0.5 to 10 h.
[0017] Preferably, in step three, the composite slab is subjected to continuous annealing to remove the surface oxide scale. It is first heated to 650°C to 750°C to recrystallize the core titanium plate, and then heated to 620°C to 720°C to recrystallize the titanium palladium acid-corroded metal alloy plate.
[0018] Preferably, the hot-rolled coil is straightened or sandblasted and pickled after annealing to achieve an overall flatness of ≤5mm / m.
[0019] The present invention has the following beneficial effects:
[0020] (1) By preparing titanium-based titanium-palladium metal composite plates, the sandblasting and hot straightening steps in the titanium electrode preparation process can be omitted, which greatly shortens the titanium electrode preparation cycle, reduces the titanium electrode preparation cost, and improves the titanium electrode preparation efficiency.
[0021] (2) In contrast to traditional electrodes, the titanium substrate is oxidized by active oxygen to form a TiO2 passivation layer, which leads to electrode failure. The titanium-based titanium-palladium metal composite plate of the present invention contains palladium, a noble metal with strong oxidation resistance and corrosion resistance, which can greatly increase the oxidation resistance of the titanium substrate and thus improve the durability of the titanium electrode.
[0022] (3) Compared with traditional mechanical sandblasting, which cannot guarantee the uniformity of roughness of sandblasted titanium substrate, this invention combines titanium plate and titanium palladium acid-corroded metal alloy plate, and then treats it with acid (hydrochloric acid, sulfuric acid or boiling oxalic acid) to completely dissolve the acid-corroded metal, so as to directly obtain a porous titanium-based titanium palladium metal composite plate with uniform roughness suitable for titanium electrode preparation.
[0023] (4) Compared with traditional sandblasting pressure, which makes the flatness of the substrate worse, and high-temperature heat straightening causes the microstructure of titanium material to change significantly, affecting the life of titanium electrode; the present invention can directly obtain titanium-based titanium-palladium metal composite plate with high flatness without heat straightening, ensuring that the microstructure of titanium substrate does not change and ensuring the performance of titanium electrode. Attached Figure Description
[0024] Figure 1 This is a schematic diagram of the method steps of the present invention.
[0025] Among them: 1. Titanium plate; 2. Titanium palladium acid etched metal alloy plate; 3. Titanium-based titanium palladium metal composite plate. Detailed Implementation
[0026] The present invention will now be described in detail with reference to the accompanying drawings. The present invention provides a technical solution: a method for preparing a titanium substrate that can shorten the titanium electrode preparation process, such as... Figure 1 This includes the following steps:
[0027] Step 1: Preparation of Titanium Plate 1: Sponge titanium of grade 0 or higher is pressed and then welded into electrodes under vacuum. The pressed plates are then smelted to obtain a uniformly composed ingot. The ingot is peeled, machined, and ultrasonically tested to grade B or higher. After forging and shaping, a titanium slab with a fragmented and uniform microstructure is obtained, with a thickness of 120–200 mm. The titanium slab is rolled using a reversible rolling mill into coils with a thickness of 3–5 mm. After annealing at 650℃–750℃, shot peening and pickling are performed to remove the oxide scale, resulting in a grain size of grade 6–10 with uniform grains. Hot-rolled coils are rolled in multiple passes with a deformation of ≤12% per pass and a rolling deformation of 30%–55% per stroke. The rolling speed is 50–180 m / min. The sheet shape is well controlled during rolling. Then, annealing is performed at a temperature of 620–720℃ and a holding time of 0.5–10 h. The annealing can be performed in a vacuum bell furnace or by cutting the annealed billet into plates, stacking them, pressing and straightening them, and then performing atmospheric annealing. After vacuum bell furnace annealing, straightening is performed. After atmospheric annealing, sandblasting and pickling are performed to achieve an overall flatness of ≤5 mm / m and obtain a good sheet shape.
[0028] Step 2: Preparation of Titanium Palladium Acid-Etched Metal Alloy Plate 2: Sponge titanium of grade 0 or higher, palladium powder with a purity of not less than 99.9%, and at least one acid-corroding metal powder are mixed and pressed. The palladium content is approximately 0.06%-0.08%, and the acid-corroding metal content is 1.00%-15.20%. The acid-corroding metal is a metal that can be corroded by acid. The acid-corroding metal powder can be one of the following metals: iron, calcium, magnesium, zinc, nickel, or an alloy of several of them. After pressing, the powder is welded into electrodes under vacuum. The electrodes are then smelted to obtain a uniformly composed ingot. After peeling and polishing the ingot, it is forged and shaped to obtain a titanium palladium acid-corroded metal composite plate blank with a fragmented and uniform as-cast structure. The thickness of the obtained titanium palladium acid-corroded metal composite plate blank is 20-80 mm. Titanium palladium acid-corroded metal composite slabs are rolled using a reversible rolling mill to produce coils with a thickness of 0.5 mm to 1 mm. After annealing at 650℃ to 750℃, the surface oxide scale is removed by shot blasting and pickling to obtain hot-rolled coils with a grain size of 8 to 10 and uniform grain size. The hot-rolled coils are then subjected to multi-pass rolling with a pass deformation of ≤12% and a rolling stroke deformation of 30% to 55%, at a rolling speed of 50 to 180 m / min. Annealing is then performed at a temperature of 620 to 720℃ and a holding time of 0.5 to 10 h. Annealing can be performed using a vacuum bell furnace or by cutting the annealed slabs into plates, stacking them, pressing them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening is performed, followed by sandblasting and pickling to achieve an overall plate unevenness of ≤5 mm / m and obtain a good plate shape.
[0029] Step 3: Preparation of Titanium-Based Titanium-Palladium Metal Composite Plate 3: The titanium plate 1 prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate 2 prepared in Step 2 are assembled into a billet. At least one titanium-palladium acid-etched metal alloy plate 2 is combined on both the top and bottom surfaces of each titanium plate 1. This can be combined into a multi-layer composite billet of titanium-titanium-palladium acid-etched metal alloy or titanium-titanium-palladium acid-etched metal alloy. The assembled billet is composited by rolling or explosive composite. The composite billet is then annealed and pickled to remove the surface oxide scale using a continuous annealing and pickling line. It is first heated to 650℃~750℃ to recrystallize the core titanium plate 1. The annealing time is calculated based on the thickness of the titanium plate 1. Then it is heated to 620℃~ At 720℃, the titanium-palladium acid-corroded metal alloy plate 2 recrystallizes. Finally, the formed composite plate is immersed in an acid solution. The surface layer of the composite plate (2-5μm) contains uniform acid-corroded metal elements. The acid-corroded metal is easily dissolved in the acid solution. The preferred acid is hydrochloric acid, sulfuric acid, oxalic acid, phosphoric acid, etc. By immersing the cut composite plate in the acid solution for a certain period of time until the acid-corroded metal is completely dissolved, a porous titanium-based titanium-palladium metal composite plate 3 is obtained. The titanium-based titanium-palladium metal composite plate 3 obtained in this way has a uniform surface roughness and high flatness, which can reduce the titanium electrode preparation production process (sandblasting and shaping), greatly shorten the electrode preparation cycle, reduce the electrode preparation cost, and improve the electrode preparation efficiency.
[0030] The present invention will be further described in detail below with reference to embodiments:
[0031] Example 1:
[0032] Step 1: Titanium Plate Preparation: Sponge titanium of grade 0 or higher is pressed and then welded into electrodes under vacuum. The pressed titanium is then smelted to obtain a uniformly composed ingot. The ingot is peeled, machined, and ultrasonically tested to grade B or higher. After forging and shaping, a titanium slab blank with a thickness of 120–200 mm is obtained. The titanium slab blank is rolled using a reversible rolling mill into a coil with a thickness of 3–5 mm. After annealing at 650–750℃, it is shot-peened and pickled to obtain a hot-rolled coil. The hot-rolled coil is then further processed… Multi-pass rolling is performed, with a pass deformation of ≤12% and a rolling stroke deformation of 30%–55%. The rolling speed is 50–180 m / min. The plate shape is well controlled during rolling, followed by annealing. The annealing temperature is 620–720℃, and the holding time is 0.5–10 h. The annealing treatment can be carried out by vacuum bell furnace annealing or by cutting the annealed billet into plates, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening treatment is performed. After atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5 mm / m.
[0033] Step Two: Preparation of Titanium Palladium Acid-Corroded Metal Alloy Plate 2: Sponge titanium of grade 0 or higher, palladium powder with a purity of not less than 99.9%, and at least one acid-corroding metal powder are mixed and pressed. The palladium content is approximately 0.06%-0.08%, and the acid-corroding metal content is 1.00%-1.02%. After pressing, the plates are welded into electrodes under vacuum. The electrodes are then melted to obtain a uniformly composed ingot. After peeling and polishing the ingot, it is forged and shaped to obtain a titanium palladium acid-corroded metal composite plate blank. Multiple tests and verifications of the titanium palladium acid-corroded metal composite plate blank confirm that the palladium content is approximately 0.06%-0.08%, and the acid-corroding metal content is 1.00%-1.02%, indicating a qualified plate blank. The obtained titanium palladium acid-corroded metal composite plate... The thickness of the composite slab is 20-80mm. The titanium palladium acid-corroded metal composite slab is rolled using a reversible rolling mill to produce coils with a thickness of 0.5mm-1mm. After annealing at 650℃-750℃, it is shot-blasted and pickled to obtain hot-rolled coils. The hot-rolled coils are rolled in multiple passes with a deformation of ≤12% per pass and a deformation of 30%-55% per rolling stroke at a rolling speed of 50-180m / min. Then, they are annealed at 620-720℃ for 0.5-10h. The annealing can be carried out in a vacuum bell furnace or by cutting the annealed billet into slabs, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening is performed, and after atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5mm / m.
[0034] Step 3: Preparation of Titanium-Based Titanium-Palladium Metal Composite Plate 3: The titanium plate 1 prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate 2 prepared in Step 2 are assembled into a multi-layer composite billet of titanium-titanium-palladium acid-etched metal alloy or titanium-titanium-palladium acid-etched metal alloy. The composite billet is composited by rolling or explosive composite. The composite billet is annealed and pickled using a continuous annealing and pickling line. First, it is heated to 650℃~750℃ to recrystallize the core titanium plate 1. The annealing time is calculated according to the thickness of titanium plate 1. Then, it is heated to 620~720℃ to recrystallize the titanium-palladium acid-etched metal alloy plate 2. Finally, the formed composite plate is immersed in an acid solution. The surface layer of the composite plate (2-5μm) contains uniform acid-etched metal elements, which are easily dissolved in the acid solution. By immersing the cut composite plate in the acid solution for a certain period of time until the acid-etched metal is completely dissolved, a porous titanium-based titanium-palladium metal composite plate 3 is obtained.
[0035] Example 2:
[0036] Step 1: Titanium Plate Preparation: Sponge titanium of grade 0 or higher is pressed and then welded into electrodes under vacuum. The pressed titanium is then smelted to obtain a uniformly composed ingot. The ingot is peeled, machined, and ultrasonically tested to grade B or higher. After forging and shaping, a titanium slab blank with a thickness of 120–200 mm is obtained. The titanium slab blank is rolled using a reversible rolling mill into a coil with a thickness of 3–5 mm. After annealing at 650–750℃, it is shot-peened and pickled to obtain a hot-rolled coil. The hot-rolled coil is then further processed… Multi-pass rolling is performed, with a pass deformation of ≤12% and a rolling stroke deformation of 30%–55%. The rolling speed is 50–180 m / min. The plate shape is well controlled during rolling, followed by annealing. The annealing temperature is 620–720℃, and the holding time is 0.5–10 h. The annealing treatment can be carried out by vacuum bell furnace annealing or by cutting the annealed billet into plates, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening treatment is performed. After atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5 mm / m.
[0037] Step Two: Preparation of Titanium Palladium Acid-Corroded Metal Alloy Plate 2: Sponge titanium of grade 0 or higher, palladium powder with a purity of not less than 99.9%, and at least one acid-corroding metal powder are mixed and pressed. The palladium content is approximately 0.06%-0.08%, and the acid-corroding metal content is 5.00%-5.20%. After pressing, the plates are welded into electrodes under vacuum. The electrodes are then melted to obtain a uniformly composed ingot. After peeling and polishing the ingot, it is forged and shaped to obtain a titanium palladium acid-corroded metal composite plate blank. Multiple tests and verifications of the titanium palladium acid-corroded metal composite plate blank confirm that the palladium content is approximately 0.06%-0.08% and the acid-corroding metal content is 5.00%-5.20%, indicating a qualified plate blank. The obtained titanium palladium acid-corroded metal composite plate... The thickness of the composite slab is 20-80mm. The titanium palladium acid-corroded metal composite slab is rolled using a reversible rolling mill to produce coils with a thickness of 0.5mm-1mm. After annealing at 650℃-750℃, it is shot-blasted and pickled to obtain hot-rolled coils. The hot-rolled coils are rolled in multiple passes with a deformation of ≤12% per pass and a deformation of 30%-55% per rolling stroke at a rolling speed of 50-180m / min. Then, they are annealed at 620-720℃ for 0.5-10h. The annealing can be carried out in a vacuum bell furnace or by cutting the annealed billet into slabs, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening is performed, and after atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5mm / m.
[0038] Step 3: Preparation of Titanium-Based Titanium-Palladium Metal Composite Plate 3: The titanium plate 1 prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate 2 prepared in Step 2 are assembled into a multi-layer composite billet of titanium-titanium-palladium acid-etched metal alloy or titanium-titanium-palladium acid-etched metal alloy. The composite billet is composited by rolling or explosive composite. The composite billet is annealed and pickled using a continuous annealing and pickling line. First, it is heated to 650℃~750℃ to recrystallize the core titanium plate 1. The annealing time is calculated according to the thickness of titanium plate 1. Then, it is heated to 620~720℃ to recrystallize the titanium-palladium acid-etched metal alloy plate 2. Finally, the formed composite plate is immersed in an acid solution. The surface layer of the composite plate (2-5μm) contains uniform acid-etched metal elements, which are easily dissolved in the acid solution. By immersing the cut composite plate in the acid solution for a certain period of time until the acid-etched metal is completely dissolved, a porous titanium-based titanium-palladium metal composite plate 3 is obtained.
[0039] Example 3:
[0040] Step 1: Titanium Plate Preparation: Sponge titanium of grade 0 or higher is pressed and then welded into electrodes under vacuum. The pressed titanium is then smelted to obtain a uniformly composed ingot. The ingot is peeled, machined, and ultrasonically tested to grade B or higher. After forging and shaping, a titanium slab blank with a thickness of 120–200 mm is obtained. The titanium slab blank is rolled using a reversible rolling mill into a coil with a thickness of 3–5 mm. After annealing at 650–750℃, it is shot-peened and pickled to obtain a hot-rolled coil. The hot-rolled coil is then further processed… Multi-pass rolling is performed, with a pass deformation of ≤12% and a rolling stroke deformation of 30%–55%. The rolling speed is 50–180 m / min. The plate shape is well controlled during rolling, followed by annealing. The annealing temperature is 620–720℃, and the holding time is 0.5–10 h. The annealing treatment can be carried out by vacuum bell furnace annealing or by cutting the annealed billet into plates, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening treatment is performed. After atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5 mm / m.
[0041] Step Two: Preparation of Titanium Palladium Acid-Etched Metal Alloy Plate 2: Sponge titanium of grade 0 or higher, palladium powder with a purity of not less than 99.9%, and at least one acid-etching metal powder are mixed and pressed. The palladium content is approximately 0.06%-0.08%, and the acid-etching metal content is 10.00%-10.20%. After pressing, the plates are welded into electrodes under vacuum. The electrodes are then melted to obtain a uniformly composed ingot. After peeling and polishing the ingot, it is forged and shaped to obtain a titanium palladium acid-etched metal composite plate blank. Multiple tests and verifications of the titanium palladium acid-etched metal composite plate blank confirm that the palladium content is approximately 0.06%-0.08%, and the acid-etching metal content is 10.00%-10.20%, indicating a qualified plate blank. The obtained titanium palladium acid-etched metal... The composite slab thickness is 20-80mm. The titanium palladium acid-corroded metal composite slab is rolled using a reversible rolling mill to produce coils with a thickness of 0.5mm-1mm. After annealing at 650℃-750℃, it is shot-blasted and pickled to obtain hot-rolled coils. The hot-rolled coils are rolled in multiple passes with a deformation of ≤12% per pass and a deformation of 30%-55% per rolling stroke at a rolling speed of 50-180m / min. Then, annealing is performed at a temperature of 620-720℃ for a holding time of 0.5-10h. The annealing can be performed using a vacuum bell furnace or by cutting the annealed billet into slabs, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening is performed, and after atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5mm / m.
[0042] Step 3: Preparation of Titanium-Based Titanium-Palladium Metal Composite Plate 3: The titanium plate 1 prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate 2 prepared in Step 2 are assembled into a multi-layer composite billet of titanium-titanium-palladium acid-etched metal alloy or titanium-titanium-palladium acid-etched metal alloy. The composite billet is composited by rolling or explosive composite. The composite billet is annealed and pickled using a continuous annealing and pickling line. First, it is heated to 650℃~750℃ to recrystallize the core titanium plate 1. The annealing time is calculated according to the thickness of titanium plate 1. Then, it is heated to 620~720℃ to recrystallize the titanium-palladium acid-etched metal alloy plate 2. Finally, the formed composite plate is immersed in an acid solution. The surface layer of the composite plate (2-5μm) contains uniform acid-etched metal elements, which are easily dissolved in the acid solution. By immersing the cut composite plate in the acid solution for a certain period of time until the acid-etched metal is completely dissolved, a porous titanium-based titanium-palladium metal composite plate 3 is obtained.
[0043] Example 4:
[0044] Step 1: Titanium Plate Preparation: Sponge titanium of grade 0 or higher is pressed and then welded into electrodes under vacuum. The pressed titanium is then smelted to obtain a uniformly composed ingot. The ingot is peeled, machined, and ultrasonically tested to grade B or higher. After forging and shaping, a titanium slab blank with a thickness of 120–200 mm is obtained. The titanium slab blank is rolled using a reversible rolling mill into a coil with a thickness of 3–5 mm. After annealing at 650–750℃, it is shot-peened and pickled to obtain a hot-rolled coil. The hot-rolled coil is then further processed… Multi-pass rolling is performed, with a pass deformation of ≤12% and a rolling stroke deformation of 30%–55%. The rolling speed is 50–180 m / min. The plate shape is well controlled during rolling, followed by annealing. The annealing temperature is 620–720℃, and the holding time is 0.5–10 h. The annealing treatment can be carried out by vacuum bell furnace annealing or by cutting the annealed billet into plates, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening treatment is performed. After atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5 mm / m.
[0045] Step Two: Preparation of Titanium Palladium Acid-Etched Metal Alloy Plate 2: Sponge titanium of grade 0 or higher, palladium powder with a purity of not less than 99.9%, and at least one acid-etching metal powder are mixed and pressed. The palladium content is approximately 0.06%-0.08%, and the acid-etching metal content is 15.00%-15.20%. After pressing, the plates are welded into electrodes under vacuum. The electrodes are then melted to obtain a uniformly composed ingot. After peeling and polishing the ingot, it is forged and shaped to obtain a titanium palladium acid-etched metal composite plate blank. Multiple tests and verifications of the titanium palladium acid-etched metal composite plate blank confirm that the palladium content is approximately 0.06%-0.08%, and the acid-etching metal content is 15.00%-15.20%, indicating a qualified plate blank. The obtained titanium palladium acid-etched metal... The composite slab thickness is 20-80mm. The titanium palladium acid-corroded metal composite slab is rolled using a reversible rolling mill to produce coils with a thickness of 0.5mm-1mm. After annealing at 650℃-750℃, it is shot-blasted and pickled to obtain hot-rolled coils. The hot-rolled coils are rolled in multiple passes with a deformation of ≤12% per pass and a deformation of 30%-55% per rolling stroke at a rolling speed of 50-180m / min. Then, annealing is performed at a temperature of 620-720℃ for a holding time of 0.5-10h. The annealing can be performed using a vacuum bell furnace or by cutting the annealed billet into slabs, stacking them, pressing and straightening them, and then atmospheric annealing. After vacuum bell furnace annealing, straightening is performed, and after atmospheric annealing, sandblasting and pickling are performed to achieve an overall plate flatness of ≤5mm / m.
[0046] Step 3: Preparation of Titanium-Based Titanium-Palladium Metal Composite Plate 3: The titanium plate 1 prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate 2 prepared in Step 2 are assembled into a multi-layer composite billet of titanium-titanium-palladium acid-etched metal alloy or titanium-titanium-palladium acid-etched metal alloy. The composite billet is composited by rolling or explosive composite. The composite billet is annealed and pickled using a continuous annealing and pickling line. First, it is heated to 650℃~750℃ to recrystallize the core titanium plate 1. The annealing time is calculated according to the thickness of titanium plate 1. Then, it is heated to 620~720℃ to recrystallize the titanium-palladium acid-etched metal alloy plate 2. Finally, the formed composite plate is immersed in an acid solution. The surface layer of the composite plate (2-5μm) contains uniform acid-etched metal elements, which are easily dissolved in the acid solution. By immersing the cut composite plate in the acid solution for a certain period of time until the acid-etched metal is completely dissolved, a porous titanium-based titanium-palladium metal composite plate 3 is obtained.
[0047] The above four specific embodiments control the content of acid-etched metal during the preparation of titanium-palladium acid-etched metal alloy plate 2 to control the surface of the titanium-based titanium-palladium metal composite plate 3 to have pores of different densities and sizes, thereby obtaining different roughness and meeting the roughness requirements of electrode preparation.
[0048] The above description is a further detailed explanation of the present invention in conjunction with specific preferred embodiments. It should not be construed that the specific implementation of the present invention is limited to these descriptions. It should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention.
Claims
1. A method for preparing a titanium substrate that can shorten the preparation process of a titanium electrode, characterized in that, Includes the following steps: Step 1: Titanium plate preparation; Step 2: Preparation of Titanium Palladium Acid-Corroded Metal Alloy Plate: Titanium powder, palladium powder, and acid-corroded metal powder are mixed, pressed, and welded into electrodes. The electrodes are melted into ingots, and the ingots are forged and shaped into titanium palladium acid-corroded metal composite blanks. The titanium palladium acid-corroded metal composite blanks are rolled and annealed to obtain hot-rolled coils with a grain size of 8-10 and uniform grain size. The hot-rolled coils are then rolled and annealed to become titanium palladium acid-corroded metal alloy plates, wherein the palladium content is 0.06%-0.08%, and the acid-corroded metal content is 1.00%-15.20%. The acid-corroded metal is a metal that can be corroded by acid. Step 3: Preparation of titanium-based titanium-palladium metal composite plate: The titanium plate prepared in Step 1 and the titanium-palladium acid-etched metal alloy plate prepared in Step 2 are assembled into a blank, with at least one side of the titanium plate being composited with the titanium-palladium acid-etched metal alloy plate. Then, the surface oxide scale is removed by annealing. Finally, the formed composite plate is immersed in an acid solution until the acid-etched metal is completely dissolved to obtain a porous titanium-based titanium-palladium metal composite plate.
2. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 1, characterized in that, The titanium plate preparation in step one is as follows: titanium powder is pressed and welded into electrodes, the electrodes are melted into ingots, the ingots are forged and shaped into titanium plate blanks with fragmented and uniform as-cast structure, the titanium plate blanks are rolled and annealed to obtain hot-rolled coils with a grain size of 6-10 and uniform grain size, and the hot-rolled coils are then rolled and annealed to become titanium plates.
3. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 2, characterized in that, In step one, the thickness of the titanium slab is 120-200 mm.
4. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 2, characterized in that, In step one, the titanium slab is rolled into a coil with a thickness of 3mm to 5mm, and after annealing at 650℃ to 750℃, the oxide scale is removed to obtain a hot-rolled coil.
5. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 2, characterized in that, In step one, the hot-rolled coil is rolled in multiple passes with a deformation amount of ≤12% per pass, a rolling deformation amount of 30% to 55% per stroke, and a rolling speed of 50 to 180 m / min; then it is annealed at a temperature of 620 to 720℃ and a holding time of 0.5 to 10 h.
6. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 1, characterized in that, The thickness of the titanium palladium acid-corroded metal composite slab obtained in step two is 20-80 mm.
7. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 1, characterized in that, In step two, the titanium palladium acid-etched metal composite slab is rolled into a coil with a thickness of 0.5 mm to 1 mm, and after annealing at 650℃ to 750℃, the surface oxide scale is removed to obtain a hot-rolled coil.
8. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 1, characterized in that, In step two, the hot-rolled coil is rolled in multiple passes with a deformation amount of ≤12% per pass, a deformation amount of 30% to 55% per rolling stroke, and a rolling speed of 50 to 180 m / min; then it is annealed at a temperature of 620 to 720℃ for a holding time of 0.5 to 10 h.
9. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to claim 1, characterized in that, In step three, the composite slab is continuously annealed to remove the surface oxide scale. It is first heated to 650℃~750℃ to recrystallize the core titanium plate, and then heated to 620~720℃ to recrystallize the titanium palladium acid-corroded metal alloy plate.
10. The method for preparing a titanium substrate that can shorten the titanium electrode preparation process according to any one of claims 5 and 8, characterized in that, After annealing, hot-rolled coils are straightened or sandblasted and pickled to achieve an overall flatness of ≤5mm / m.