CN112877656A - Zirconium tube target and production method thereof - Google Patents
Zirconium tube target and production method thereof Download PDFInfo
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- CN112877656A CN112877656A CN202110025644.6A CN202110025644A CN112877656A CN 112877656 A CN112877656 A CN 112877656A CN 202110025644 A CN202110025644 A CN 202110025644A CN 112877656 A CN112877656 A CN 112877656A
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- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 69
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000004513 sizing Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 11
- 238000005097 cold rolling Methods 0.000 claims abstract description 10
- 238000005098 hot rolling Methods 0.000 claims abstract description 10
- 238000010891 electric arc Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000005498 polishing Methods 0.000 claims description 15
- 238000005096 rolling process Methods 0.000 claims description 13
- 238000005242 forging Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 10
- 238000007514 turning Methods 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 230000007547 defect Effects 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000003754 machining Methods 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000003754 zirconium Chemical class 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229910052580 B4C Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019580 granularity Nutrition 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000001579 optical reflectometry Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a zirconium tube target and a production method, which comprises a zirconium tube main body, wherein the zirconium tube main body is a hollow cylindrical structure, two ends of the zirconium tube main body are respectively provided with a pair of bell mouth grooves with annular structures, and the end parts of the bell mouth grooves are symmetrically provided with limit rings with annular groove structures, the zirconium tube target has the advantages that the zirconium tube target selects high-quality sponge zirconium, adopts an electric arc furnace which is specially used for smelting zirconium materials with the volume of more than 3 tons and strictly cleans a furnace hearth, so that the pollution of other impurities in the smelting process is avoided, the deformation rate exceeds 93 percent in the processes of perforation, hot rolling and sizing, the structure is uniform, the crystal grains are fine, the performance is excellent, 20000-plus-50000 mm long tubes can be produced, the yield is greatly improved, the yield from a bar blank to the tube can reach 98 percent, the efficiency is high, only 8 to 10 minutes are needed for producing the 20000-plus-50000 mm tube, and the grains can be further refined by adopting cold rolling forming. Each shift can produce 15-30 tons of zirconium tubes.
Description
Technical Field
The invention relates to the technical field of zirconium tube targets, in particular to a zirconium tube target and a production method thereof.
Background
Zirconium is widely used in coating films of chemical equipment, display screens and various tools due to excellent corrosion resistance and high light reflectivity. With the development of the coating technology, the usage amount of the vacuum magnetron sputtering rotating tube target is larger and larger. The conventional zirconium tube target is produced by extrusion molding, and is difficult to make a large-diameter super-long tube due to the limitation of extrusion force of an extruder, the diameter of an extrusion cylinder and the length. Typically the length of the extrusion is not more than 6 metres. And because the extrusion needs to be coated and lubricated by a copper coating sleeve, the extrusion surface is not smooth, and the coated copper is removed by an acid pickling method. Serious pollution, high production cost and low efficiency, and the scheme is generated by the intensive research aiming at the problems.
Disclosure of Invention
The invention aims to solve the problems, designs a zirconium tube target and a production method thereof, and solves the problems of the prior art.
The technical scheme of the invention for realizing the aim is as follows: the utility model provides a zirconium tube target, includes zirconium tube main part, zirconium tube main part is the cylindrical structure of cavity, zirconium tube main part both ends are seted up the bellmouth groove of a pair of annular structure respectively, and is a pair of bellmouth groove tip symmetry sets up the spacing ring of annular groove structure.
And the inner rings at the two ends of the zirconium tube main body are respectively provided with an annular groove with an inclination angle of 25 degrees with the horizontal direction.
The thinnest wall surface thickness of the zirconium tube main body is not less than 0.3 mm.
A production method of a zirconium tube target comprises the following steps: step S1, smelting and forging, step S2, annealing and turning, step S3, perforating, hot continuous rolling and sizing, step S4, blanking straightening, step S5, internal and external surface treatment, step S6, cold rolling, step S7, heat treatment, step S8, honing, step S9, machining, step S10 and polishing treatment;
step S1: HZr-1 high-quality sponge zirconium pressing electrode according with national standard is adopted, smelting is carried out for 2-3 times in an electric arc furnace specially used for smelting zirconium materials with the capacity of more than 3 tons, a smelted cast ingot is forged on a press, three piers and three pulls are carried out on the cast ingot, and the cogging temperature is as follows: 900 ℃ -1100 ℃, secondary-fire precision forging temperature: precisely forging the alloy into a phi 205 precisely-forged rod at the temperature of 700 ℃ and 900 ℃;
step S2: annealing the finish forging rod, interrupting and peeling, turning off an oxide layer of an excircle, and turning a through hole at one end;
step S3: hot continuous rolling and sizing are carried out through perforation, a 180 steel rolling mill set is modified, an electric furnace heating system is added, the radian of a perforation guide plate is designed and trimmed, a high-strength chrome-molybdenum alloy steel top head is adopted as the top head, a hot rolling mill set is modified to be easy to bite into a tube blank, an induction heat supplementing system is added in front of the sizing mill set, and a plurality of sizing rollers with different diameters are adopted for hot sizing;
step S4: cutting and blanking the pipe subjected to hot rolling and sizing and straightening;
step S5: polishing the inner hole of the pipe after hot rolling, sizing and straightening, peeling on an outer diameter peeling machine, and removing an oxide layer and surface defects;
step S6: performing multi-pass cold rolling on the processed tube blank according to the size requirement;
step S7: carrying out recrystallization vacuum heat treatment in a vacuum heat treatment furnace, wherein the heat treatment system comprises the following steps: heating temperature: 600 ℃ and 800 ℃, preserving the heat for 1-3 hours, wherein the vacuum degree is as follows: cooling the furnace to be below 100 ℃ under 10-3Pa, and discharging the furnace;
step S8: honing an inner hole of the inner circle of the heat-treated zirconium tube on a honing machine according to the drawing requirements, wherein the honing abrasive strip adopts an abrasive strip with medium hardness, the grinding amount is about 0.2-0.7mm, and the roughness is less than 1.6 microns;
step S9: honing the zirconium pipe with the inner hole, turning the outer diameter and branch ports at two ends according to the requirements of a drawing, and designing an intermediate supporting device for a longer pipe;
step S10: the machined pipe is polished, a polishing clamping system is designed, and abrasive belts with different particle sizes and nylon polishing cloth are adopted for multi-pass polishing, so that the surface roughness of the pipe is less than 1.6 microns and can reach 0.5 micron at most.
The cogging temperature in the step S1 is preferably set to 1000-1050 ℃, and the two-fire finish forging temperature is preferably set to 800-850 ℃.
The deformation rate of the cold rolling in the step S6 is more than or equal to 40 percent.
In step S7, before the heat treatment, the rolled zirconium tube is first subjected to oleic acid removal and then washed.
The heating temperature in step S7 is preferably set at 650-750 deg.C, and the temperature is maintained for 1.5-2.5 hours.
In the step S8, the honing abrasive strip with medium hardness is adopted, and the grinding amount is about 0.3-0.6 mm.
And (S10) polishing the machined pipe, and performing polishing treatment for at least 3 times by adopting abrasive belts and nylon polishing cloth with different granularities.
The zirconium tube target manufactured by the technical scheme of the invention selects high-quality sponge zirconium, adopts an electric arc furnace specially used for smelting zirconium materials with the volume of more than 3 tons, strictly cleans a furnace hearth, avoids pollution of other impurities in the smelting process, particularly Ti, ensures that the chemical composition of the cast ingot meets the standard requirement, strictly controls the heat deformation rate during forging, carries out 2-3 times of upsetting during cogging of the cast ingot, greatly crushes crystal grains, and adopts a special oblique rolling perforation hot continuous rolling and hot sizing process, wherein the total deformation rate of the cast ingot reaches more than 90 percent. In the processes of perforation, hot rolling and sizing, the deformation rate exceeds 93 percent, so that the structure is uniform, the crystal grains are fine, the performance is excellent, 20000-plus-50000 mm long pipes can be produced, the yield is greatly improved, the yield from a bar blank to the pipe can reach 98 percent, the efficiency is high, only 8 to 10 minutes are needed for producing one 20000-plus-50000 mm pipe, and the crystal grains can be further refined by adopting cold rolling forming. Each shift can produce 15-30 tons of zirconium tubes.
Drawings
FIG. 1 is a schematic structural diagram of a zirconium tube target and a production method thereof according to the present invention.
FIG. 2 is a schematic side view of a zirconium tube target and a method for producing the same according to the present invention.
FIG. 3 is a schematic diagram of a partially enlarged structure of a zirconium tube target and a method for producing the same according to the present invention.
In the figure: 1. a zirconium tube body; 2. a socket groove; 3. a limiting ring; 4. and (4) annular groove preparation.
Detailed Description
The present invention is specifically described below with reference to the accompanying drawings, and as shown in fig. 1 to 3, the present embodiment is characterized by comprising a zirconium tube main body 1, wherein the zirconium tube main body 1 is a cylindrical structure with a cavity, two ends of the zirconium tube main body 1 are respectively provided with a pair of socket grooves 2 with an annular structure, and the end portions of the pair of socket grooves 2 are symmetrically provided with a spacing ring 3 with an annular groove structure; this zirconium tube target has selected high-quality sponge zirconium for use, adopts the electric arc furnace of smelting the zirconium material specially more than 3 tons to carry out strict clearance to the furnace hearth, avoided the pollution of other impurity among the melting process, especially Ti, make its ingot casting chemical composition accord with the standard requirement, strict control heat deformation rate during forging has carried out 2-3 times mounds and has pulled out when cogging to its ingot casting, the crystalline grain has been broken to the very big degree, its total deformation rate has reached more than 90%, adopt special cross rolling perforation hot continuous rolling, hot sizing technology. In the processes of perforation, hot rolling and sizing, the deformation rate exceeds 93 percent, so that the structure is uniform, the crystal grains are fine, the performance is excellent, 20000-plus-50000 mm long pipes can be produced, the yield is greatly improved, the yield from a bar blank to the pipe can reach 98 percent, the efficiency is high, only 8 to 10 minutes are needed for producing one 20000-plus-50000 mm pipe, and the crystal grains can be further refined by adopting cold rolling forming. Each shift can produce 15-30 tons of zirconium tubes.
The following working principles, detailed connecting means thereof, and the following main descriptions of the working principles and processes are well known in the art, and will be referred to by those skilled in the art for the specific connection and operation sequence of the components in this application.
Example (b): an HZr-1-grade sponge zirconium pressing electrode which meets the national standard and has the best quality is purchased, an electrode rod is manufactured, three times of electric arc melting is carried out in a special 3-ton electric arc furnace, and a melted cast ingot is forged on a 3500-ton oil press. The cogging temperature is less than 1000 ℃, and three times of upsetting are carried out, the second heating temperature is less than 850 ℃, and the steel bar is processed into phi 205 x L round bar, and the total processing rate is more than or equal to 90 percent. And carrying out annealing treatment at 650-700 ℃ on the forged round rod. The heat treated forged bars were interrupted and scalped and a phi 70 x 70 pilot hole was turned at one end to produce phi 200 x 4000mm bar stock. Heating the zirconium bar blank in a resistance furnace, wherein the heating temperature is as follows: keeping the temperature for 4-6 hours at 850-980 ℃. The heated billets were transferred to a 4700 ton cross piercing mill for cross piercing. And spraying boron carbide lubrication in the perforated zirconium pipe, transmitting the lubricated zirconium pipe to a hot rolling mill, biting a pipe head into the core rod, penetrating the core rod into the pipe hole, and carrying out hot continuous rolling. The rolled tube blank is conveyed to an induction heat supplementing system for rapid heat supplement, and the heat supplementing temperature is as follows: and (4) continuously conveying the steel plate to a sizing roller for sizing at 900 ℃, and sizing by adopting a plurality of rollers. And (4) interrupting the sized zirconium pipe. And then polishing the broken inner hole of the pipe, peeling the outer circle on a peeling machine, and removing the oxide layer and the inner and outer surface defects. Annealing treatment is carried out in a tubular vacuum annealing furnace, wherein the annealing temperature is as follows: 600 ℃ and 750 ℃ and keeping the temperature for 1.5-2.5 hours. And rolling the annealed zirconium pipe in an LG120 cold rolling mill set, and rolling in different passes according to different specifications. The rolled tube blank is degreased and pickled, and is subjected to vacuum recrystallization annealing at the annealing temperature of 680-750 ℃, the temperature is kept for 1.5-2 hours, and the annealed zirconium tube is sent to a honing machine to hone an inner hole with the roughness of 1.6-3.2 microns. The honed pipe is cut off as required and sent to a machine tool to machine the excircle and branch mouths at two ends. The processed zirconium tube is polished to a surface roughness of less than 1.6 microns. The roughness of the sealing surface of the branch port is less than 0.8 micron. And (6) inspecting, packaging and warehousing. The method produces the zirconium rotary tube targets with specifications of phi 176/phi 148X 3900mm, phi 152.4/phi 125X 3852mm, phi 145/phi 125X 850mm, phi 155 & 151/phi 125X 3191mm and the tubes with specifications of phi 160 & 180 & 5-15 & 20000 & 50000 mm. The grain size is 30-60 microns. The technology can be expanded to the production of ultra-large and ultra-long zirconium pipes and pipelines, and has high efficiency, high yield and good quality.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (10)
1. The utility model provides a zirconium tube target, includes zirconium tube main part (1), its characterized in that, zirconium tube main part (1) is the cylindrical structure of cavity, the bellmouth groove (2) of a pair of annular structure are seted up respectively to zirconium tube main part (1) both ends, and is a pair of the spacing ring (3) of annular groove structure are seted up to bellmouth groove (2) tip symmetry.
2. The zirconium tube target as claimed in claim 1, wherein the inner rings at the two ends of the zirconium tube main body (1) are respectively provided with an annular groove (4) with an inclination angle of 25 ° with the horizontal.
3. A zirconium tube target according to claim 1, characterized in that the thinnest wall thickness of the zirconium tube body (1) is not less than 0.3 mm.
4. The production method of the zirconium tube target is characterized by comprising the following steps of: step S1, smelting and forging, step S2, annealing and turning, step S3, perforating, hot continuous rolling and sizing, step S4, blanking straightening, step S5, internal and external surface treatment, step S6, cold rolling, step S7, heat treatment, step S8, honing, step S9, machining, step S10 and polishing treatment;
step S1: HZr-1 high-quality sponge zirconium pressing electrode according with national standard is adopted, smelting is carried out for 2-3 times in an electric arc furnace specially used for smelting zirconium materials with the capacity of more than 3 tons, a smelted cast ingot is forged on a press, three piers and three pulls are carried out on the cast ingot, and the cogging temperature is as follows: 900 ℃ -1100 ℃, secondary-fire precision forging temperature: precisely forging the alloy into a phi 205 precisely-forged rod at the temperature of 700 ℃ and 900 ℃;
step S2: annealing the finish forging rod, interrupting and peeling, turning off an oxide layer of an excircle, and turning a through hole at one end;
step S3: hot continuous rolling and sizing are carried out through perforation, a 180 steel rolling mill set is modified, an electric furnace heating system is added, the radian of a perforation guide plate is designed and trimmed, a high-strength chrome-molybdenum alloy steel top head is adopted as the top head, a hot rolling mill set is modified to be easy to bite into a tube blank, an induction heat supplementing system is added in front of the sizing mill set, and a plurality of sizing rollers with different diameters are adopted for hot sizing;
step S4: cutting and blanking the pipe subjected to hot rolling and sizing and straightening;
step S5: polishing the inner hole of the pipe after hot rolling, sizing and straightening, peeling on an outer diameter peeling machine, and removing an oxide layer and surface defects;
step S6: performing multi-pass cold rolling on the processed tube blank according to the size requirement;
step S7: carrying out recrystallization vacuum heat treatment in a vacuum heat treatment furnace, wherein the heat treatment system comprises the following steps: heating temperature: 600 ℃ and 800 ℃, preserving the heat for 1-3 hours, wherein the vacuum degree is as follows: cooling the furnace to be below 100 ℃ under 10-3Pa, and discharging the furnace;
step S8: honing an inner hole of the inner circle of the heat-treated zirconium tube on a honing machine according to the drawing requirements, wherein the honing abrasive strip adopts an abrasive strip with medium hardness, the grinding amount is about 0.2-0.7mm, and the roughness is less than 1.6 microns;
step S9: honing the zirconium pipe with the inner hole, turning the outer diameter and branch ports at two ends according to the requirements of a drawing, and designing an intermediate supporting device for a longer pipe;
step S10: the machined pipe is polished, a polishing clamping system is designed, and abrasive belts with different particle sizes and nylon polishing cloth are adopted for multi-pass polishing, so that the surface roughness of the pipe is less than 1.6 microns and can reach 0.5 micron at most.
5. The method as claimed in claim 4, wherein the cogging temperature in step S1 is preferably set to 1000-1050 ℃, and the two-fire finish forging temperature is preferably set to 800-850 ℃.
6. The method for producing a zirconium tube target as claimed in claim 4, wherein the cold rolling in step S6 has a deformation rate of 40% or more.
7. The method of claim 4, wherein the rolled zirconium tube is first subjected to acid removal and then subjected to acid removal before the heat treatment in step S7.
8. The method as claimed in claim 4, wherein the heating temperature in step S7 is preferably set at 650-750 deg.C, and the temperature is maintained for 1.5-2.5 hours.
9. The method for producing a zirconium tube target as claimed in claim 4, wherein the honing bar in the step S8 is a medium-hardness bar with a grinding amount of about 0.3-0.6 mm.
10. The method of claim 4, wherein the tube machined in step S10 is polished by using abrasive belts and nylon polishing cloth with different particle sizes for at least 3 times.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110025644.6A CN112877656B (en) | 2021-01-08 | 2021-01-08 | Zirconium tube target and production method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110025644.6A CN112877656B (en) | 2021-01-08 | 2021-01-08 | Zirconium tube target and production method thereof |
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| CN112877656B CN112877656B (en) | 2024-07-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN114770361A (en) * | 2022-03-23 | 2022-07-22 | 重庆欣维尔玻璃有限公司 | High-precision borosilicate glass tube inner diameter machining and inner wall polishing process |
| CN115896714A (en) * | 2022-12-30 | 2023-04-04 | 宝鸡市飞腾金属材料股份有限公司 | High-performance ultra-long large-sized rotating titanium tube target material for large wafer and preparation process |
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| CN112877656B (en) | 2024-07-02 |
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