CN111299969A - Production process of sputtering target copper strip with controllable grain size and performance - Google Patents
Production process of sputtering target copper strip with controllable grain size and performance Download PDFInfo
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- CN111299969A CN111299969A CN201911229694.5A CN201911229694A CN111299969A CN 111299969 A CN111299969 A CN 111299969A CN 201911229694 A CN201911229694 A CN 201911229694A CN 111299969 A CN111299969 A CN 111299969A
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Abstract
The invention relates to the technical field of copper plate and strip production processes, in particular to a production process of a sputtering target material copper plate and strip with controllable grain size and performance, which comprises the following steps: step 1, casting a copper blank; step 2, milling the surface; step 3, hot rolling, heating to 800-900 ℃, discharging, and performing 7-11 rolling passes, wherein the final rolling temperature is within 600-650 ℃; step 4, online quenching is carried out, and the temperature is quickly controlled within 200 ℃, so that the grain size is ensured to be within 70um, and the hardness is ensured to be within 100 HV; step 5, secondary face milling; 6, annealing; step 7, surface treatment; step 8, packaging; the method fully utilizes the existing equipment, and controls the Cu content to reach the standard for producing the cast ingot high-purity oxygen-free copper by casting; in the hot rolling production process, the grain size is controlled by controlling the heating temperature, the rolling pass, the final rolling temperature and the rapid quenching, and finally, the grain size uniformity and the physical properties meet the requirements of customers by means of bell jar furnace annealing, so that the production efficiency is improved, and the product quality is also improved.
Description
Technical Field
The invention relates to the technical field of copper plate and strip production processes, in particular to a production process of a sputtering target material copper plate and strip with controllable grain size and performance.
Background
At present, the production of copper strips is mainly carried out in a cast ingot hot rolling cogging mode. However, with the continuous development of industrial technology, the requirements on the quality and precision of copper strips are higher and higher, and the traditional rolling method cannot meet the requirements of high-quality copper strips. The annealing quality in the copper strip production process is poor, the parameter setting is not ideal, and the production operation is complicated, so that the produced copper strip cannot meet the production requirement.
The copper plate strip is also used for targets mostly, and because the requirements on the components, the grain size and the physical and chemical properties of the targets are higher, the requirements on blanks and forging equipment are higher for the conventional targets mainly through a production process designed by forging equipment, and compared with plate strip production, the production capacity is less, and mass production cannot be realized.
Disclosure of Invention
The invention provides a production process of a sputtering target copper strip with controllable grain size and performance, and aims to improve the original processing process by using the existing equipment, improve the product quality and improve the production efficiency.
A production process of a sputtering target copper strip with controllable grain size and performance comprises the following steps:
step 1: casting a copper blank, adding electrolytic copper into an oxygen-free copper furnace, adding phosphorus and charcoal, removing gas by bottom blowing, fishing slag, adjusting the temperature in the furnace to 1200-1250 ℃ to obtain molten copper of C10100, and transferring the molten copper to a heat preservation furnace; adding graphite particle coverage in the heat preservation furnace, and continuously adjusting components; after the copper water reaches the designated liquid level, the temperature is controlled to 1150-
At 1180 ℃, discharging the copper water into a crystallizer through a pouring pipe, casting a C10100 copper ingot at a speed of 60-80mm/min, covering with soot during casting, and casting a 220mm copper ingot;
step 2: milling a blank surface of the copper ingot prepared in the step 1 on a milling machine; through milling the face, can get rid of copper ingot impurity, mill back surface roughness control within 1.2Ra/um, promote the quality of copper ingot raw materials, be favorable to improving whole copper strips off-the-shelf product quality.
And step 3: hot rolling, namely uniformly heating the milled copper ingot prepared in the step 2 to 800-900 ℃ at a low temperature by a heating furnace, discharging, rolling by a hot rolling mill for 7-11 times to obtain the required thickness, and controlling the final rolling temperature to be within 600-650 ℃; heating in a heating furnace to the optimal hot rolling temperature of 800-900 ℃, and rolling for 7-11 times, so that the grain size distribution is more uniform microscopically, and defects such as air holes, shrinkage porosity and the like in the copper material are eliminated macroscopically to a certain degree.
Step 4, online quenching, namely online quenching is carried out on the copper strip with the finish rolling temperature of 600-650 ℃ in the step 3, and the temperature is quickly controlled within 200 ℃; so as to improve the surface hardness of the copper strip formed by rolling the copper ingot and increase the wear resistance.
Step 5, secondary surface milling is carried out on the copper strip prepared in the step 4; the surface of the copper strip is smooth, and the surface roughness is within 1.2Ra/um, so that the technical requirement of the next step is met.
Step 6, annealing, namely conveying the copper strip subjected to the secondary surface milling in the step 5 into an annealing furnace, keeping the temperature for 4-6 hours at the annealing temperature of 400 ℃, and then cooling by water and air to below 60 ℃; annealing can release the internal stress of the copper strip, increase the ductility and toughness of the material, generate a special microstructure, prevent the deformation and cracking of the workpiece, soften the workpiece for cutting, refine grains, and enable the grain size to be uniform and the hardness to be within 70HV after annealing.
Step 7, surface treatment, namely performing surface treatment on the copper strip annealed in the step 6, sequentially performing acid washing, rinsing with cold water, drying surface moisture, and finally performing polishing treatment; the acid cleaning can remove the oxide layer on the surface after the heat treatment, so that the corrosion resistance is increased, the product appearance is also improved through the polishing treatment, and the product quality is improved.
And 8, packaging, namely straightening the copper strip subjected to surface treatment in the step 7 in a manner of sequentially passing through a tension roller and a bending straightening roller, and inspecting, packaging and warehousing after sawing.
Specifically, the electrolytic copper in the step 1 is high-purity large-plate electrolytic copper, the purity of the electrolytic copper is more than 4N, and the component content of the C10100 pure copper produced in the step 1 is controlled to be more than 4N, less than or equal to 3ppm of oxygen, less than or equal to 3ppm of P, and less than or equal to 10ppm of Fe.
Specifically, the milling machine in the step 2 is a double-sided milling machine.
Specifically, the heating furnace in the step 3 adopts a stepping heating furnace for heating.
Specifically, in the step 4, the online quenching mode is large-flow high-pressure quenching.
Specifically, the annealing furnace in the step 6 is a bell jar annealing furnace.
Specifically, the polishing treatment in step 7 is 1000-mesh nylon polishing.
Compared with the prior art, the invention has the following beneficial effects:
the process provided by the invention comprises the steps of strictly half-pipe processing of high-quality electrolytic copper from raw materials through an imported oxygen-free copper furnace to cast a high-purity C10100 pure copper ingot, milling the surface of the copper ingot through a milling machine, and removing surface impurities for subsequent processing; heating the milled copper ingot to 800-900 ℃ at low temperature by a heating furnace, carrying out a rolling process, rolling for 7-11 times, finally controlling the rolling temperature within 600-650 ℃, and rapidly controlling the temperature within 200 ℃ through online quenching so as to enable the grain size to be within 70um and the hardness to be within 100 HV; flattening the surface of the previous step by secondary face milling; as is well known, annealing refers to a thermal process in which a material is exposed to high temperatures for a long period of time and then slowly cooled. The main purposes are to release stress, increase the ductility and toughness of materials, generate special microstructures and the like so as to improve or eliminate various structural defects and residual stress caused by steel in the casting, forging, rolling and welding processes, prevent the deformation and cracking of workpieces, soften the workpieces so as to carry out cutting processing, refine crystal grains and improve the structure so as to improve the mechanical property of the workpieces; the copper strip after the secondary surface milling enters an annealing furnace, annealing and heat preservation at the temperature of 400 ℃ is carried out for 4-6 hours, the temperature is 60 ℃ through water cooling or air cooling, the grain size is uniform after annealing, and the hardness is within 70 HV; then acid washing is carried out by using 15 percent sulfuric acid, washing is carried out by using cold water, surface moisture is dried, and finally polishing is carried out, wherein the polishing speed is 40 m/min; and finally, straightening the copper strip subjected to surface treatment in a mode of sequentially passing through a tension roller and a bending straightening roller, and after sawing, inspecting, packaging and warehousing. The method fully utilizes the existing equipment, controls the Cu content to reach more than 4N, the oxygen content is less than or equal to 3pp, the P content is less than or equal to 3ppm, and the Fe content is less than or equal to 10ppm for producing the cast ingot high-purity oxygen-free copper by casting; in the hot rolling production process of the stepping furnace, the grain size is controlled by controlling the heating temperature, the rolling pass, the final rolling temperature and the rapid quenching, and finally, the grain size uniformity and the physical properties meet the requirements of customers by annealing, so that the production efficiency is improved, and the product quality is also improved.
Drawings
FIG. 1 is a flow chart of a process for producing a sputtering target copper strip with controllable grain size and performance according to the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a process for producing a copper strip of a sputtering target with controllable grain size and performance comprises the following steps,
step 1: casting a copper blank, adding electrolytic copper into an oxygen-free copper furnace, adding phosphorus and charcoal, removing gas by bottom blowing, fishing slag, adjusting the temperature in the furnace to 1200-1250 ℃ to obtain molten copper of C10100, and transferring the molten copper to a heat preservation furnace; adding graphite particle coverage in the heat preservation furnace, and continuously adjusting components; after the copper water reaches the designated liquid level, controlling the temperature at 1150-1180 ℃, discharging the copper water into the crystallizer through the pouring pipe, casting a C10100 copper ingot at the speed of 60-80mm/min, covering with soot in the casting process, and casting a 220mm copper ingot; specifically, the electrolytic copper is high-purity large-plate electrolytic copper, the purity is more than 4N, the component content of the produced C10100 pure copper is controlled to be more than 4N, the oxygen content is less than or equal to 3ppm, the P content is less than or equal to 3ppm, and the Fe content is less than or equal to 10 ppm.
Step 2: milling the face, milling off the blank face with the copper ingot of step 1 preparation on milling machine, milling machine is two-sided milling machine, mills the two sides simultaneously, removes surface impurity, improves purity, through milling the face, can get rid of copper ingot impurity, mills back surface roughness control within 1.2Ra/um, promotes the quality of copper ingot raw materials, is favorable to improving whole copper strips off-the-shelf product quality.
And step 3: hot rolling, namely uniformly heating the milled copper ingot prepared in the step 2 to 800-900 ℃ at a low temperature by using a stepping heating furnace, discharging, rolling by using a two-roll reversible rolling mill for 7-11 times to obtain the required thickness, and controlling the final rolling temperature to be within 600-650 ℃; heating in a heating furnace to the optimal hot rolling temperature of 800-900 ℃, and rolling for 7-11 times, so that the grain size distribution is more uniform microscopically, and defects such as air holes, shrinkage porosity and the like in the copper material are eliminated macroscopically to a certain degree; the walking beam furnace has flexible material transportation, and can discharge all furnace burden out of the furnace when necessary; the blanks are arranged on the furnace bottom or the beam at intervals, so that the blanks can be quickly and uniformly heated; the arch steel and stick steel failures of push steel furnaces are completely eliminated, thus leaving the length of the furnace unlimited by these factors.
And 4, step 4: quenching on line, namely quenching the copper strip with the finish rolling temperature of 600-650 ℃ in the step 3, and rapidly controlling the temperature within 200 ℃, so as to ensure that the grain size reaches within 70um and the hardness reaches within 100 HV; the quenching can improve the surface hardness of the copper strip formed after the copper ingot is rolled, the wear resistance is improved, and the high-flow high-pressure quenching is carried out in an online quenching mode; the upper surface and the lower surface are sprayed with high-pressure water for cooling, and the amount of cooling water is 1600m3The high-pressure large-flow cooling water with the injection pressure of 0.2-0.4MPa can more quickly and accurately finish the quenching work.
And 5: secondary surface milling is carried out, wherein the copper strip prepared in the step 4 is subjected to secondary surface milling, and irregular surfaces appearing in the rolling process are leveled; the surface of the copper strip is smooth, and the surface roughness is within 1.2Ra/um, so that the technical requirement of the next step is met.
Step 6, annealing, namely conveying the copper strip subjected to the secondary surface milling in the step 5 into a bell jar annealing furnace, entering the bell jar furnace through the surface milling, keeping the temperature for 4-6 hours at the annealing temperature of 400 ℃, and then cooling by water and air to below 60 ℃; annealing can release the internal stress of the copper strip, increase the ductility and toughness of the material, generate a special microstructure, prevent the deformation and cracking of the workpiece, soften the workpiece for cutting, refine grains, ensure that the grain size is uniform after annealing and the hardness is within 70HV,
step 7, surface treatment, namely performing surface treatment on the copper strip annealed in the step 6, sequentially using 10-20% sulfuric acid for pickling, then washing with cold water, drying surface moisture, and finally performing polishing treatment; the acid cleaning can remove the oxide layer on the surface after the heat treatment, so that the corrosion resistance is increased, the product appearance is also improved through the polishing treatment, and the product quality is improved.
And 8, packaging, namely straightening the copper strip subjected to surface treatment in the step 7 in a mode of sequentially passing through a tension roller and a bending straightening roller to enable the flatness of the copper strip to reach 1mm/m, and after sawing, inspecting, packaging and warehousing.
The method fully utilizes the existing equipment, controls the Cu content to reach more than 4N, the oxygen content is less than or equal to 3pp, the P content is less than or equal to 3ppm, and the Fe content is less than or equal to 10ppm for producing the cast ingot high-purity oxygen-free copper by casting; in the hot rolling production process of the stepping furnace, the grain size is controlled by controlling the heating temperature, the rolling pass, the final rolling temperature and the rapid quenching, and finally, the grain size uniformity and the physical properties meet the requirements of customers by annealing, so that the production efficiency is improved, and the product quality is also improved.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A production process of a sputtering target copper strip with controllable grain size and performance is characterized by comprising the following steps:
step 1: casting a copper blank, adding electrolytic copper into an oxygen-free copper furnace, adding phosphorus and charcoal, removing gas by bottom blowing, fishing slag, adjusting the temperature in the furnace to 1200-1250 ℃ to obtain molten copper of C10100, and transferring the molten copper to a heat preservation furnace; adding graphite particle coverage in the heat preservation furnace, and continuously adjusting components; after the copper water reaches the designated liquid level, controlling the temperature at 1150-1180 ℃, discharging the copper water into the crystallizer through the pouring pipe, casting a C10100 copper ingot at the speed of 60-80mm/min, covering with soot in the casting process, and casting a 220mm copper ingot;
step 2: milling a blank surface of the copper ingot prepared in the step 1 on a milling machine;
and step 3: hot rolling, namely uniformly heating the milled copper ingot prepared in the step 2 to 800-900 ℃ at a low temperature by a heating furnace, discharging, rolling by a hot rolling mill for 7-11 times to obtain the required thickness, and controlling the final rolling temperature to be within 600-650 ℃;
and 4, step 4: quenching on line, namely quenching the copper strip with the finish rolling temperature of 600-650 ℃ in the step 3, and quickly controlling the temperature within 200 ℃;
and 5: secondary face milling is carried out, wherein the copper strip prepared in the step 4 is subjected to secondary face milling;
step 6: annealing, namely conveying the copper strip subjected to the secondary surface milling in the step 5 into an annealing furnace, keeping the temperature for 4-6 hours at the annealing temperature of 300-400 ℃, and then cooling by water and air to below 60 ℃;
and 7: surface treatment, namely performing surface treatment on the copper strip annealed in the step 6, sequentially using 10-20% sulfuric acid for pickling, then washing with cold water, drying surface moisture, and finally performing polishing treatment;
and 8: and packaging, namely straightening the copper strip subjected to surface treatment in a mode of sequentially passing through a tension roller and a bending straightening roller to enable the flatness of the copper strip to reach 1mm/m, and then cutting, inspecting, packaging and warehousing.
2. The production process of the sputtering target copper strip with controllable grain size and performance as claimed in claim 1, wherein the electrolytic copper in the step 1 is high-purity large-plate electrolytic copper, and the purity of the electrolytic copper is more than 4N; the component content of the produced C10100 pure copper is controlled to be more than 4N, the oxygen content is less than or equal to 3ppm, the P content is less than or equal to 3ppm, and the Fe content is less than or equal to 10 ppm.
3. The process for producing the sputtering target copper strip with controllable grain size and performance as claimed in claim 1, wherein the milling machine in the step 2 is a double-sided milling machine.
4. The process for producing a sputtering target copper strip with controllable grain size and performance as claimed in claim 1, wherein the heating furnace in step 3 is a step heating furnace and is rolled by a two-roll reversing mill.
5. The production process of the sputtering target copper strip with controllable grain size and performance as claimed in claim 1, wherein in the step 4, the online quenching mode is a high-flow high-pressure quenching mode.
6. The process for producing the sputtering target copper strip with controllable grain size and performance as claimed in claim 1, wherein the annealing furnace in the step 6 is a bell jar annealing furnace.
7. The process for producing a sputtering target copper strip with controllable grain size and performance as claimed in claim 1, wherein the polishing treatment in step 7 is 1000-mesh nylon polishing.
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CN111604651A (en) * | 2020-06-28 | 2020-09-01 | 沈阳有色金属加工有限公司 | Preparation method of large-size high-purity copper rotary target material |
CN113695388A (en) * | 2021-08-31 | 2021-11-26 | 山西春雷铜材有限责任公司 | Production method of copper-manganese-nickel hot rolled coil |
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Application publication date: 20200619 |