CN103215553B - Method for preparing high-purity titanium plate for use as target - Google Patents
Method for preparing high-purity titanium plate for use as target Download PDFInfo
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Abstract
The invention provides a method for preparing a high-purity titanium plate for use as a target. The method comprises the following steps of: pressing sponge titanium particles into an electrode block and then welding the electrode block into a consumable electrode; 2, performing vacuum arc remelting of the consumable electrode to obtain a cast ingot; 3, performing the primary heating treatment on the cast ingot; 4, performing upset drawing forging on the cast ingot, thereby obtaining a plate blank; 5, performing the secondary heating treatment on the plate blank; 6, rolling the plate blank, thereby obtaining a semi-finished product plate; 7, performing annealing, straightening and surface figuring on the semi-finished product plate, thereby obtaining the high-purity titanium plate for use as the target. The mass purity of the high-purity titanium plate prepared by the method provided by the invention for use as the target is not less than 99.8%, and the average grain size of the plate is less than 100 microns; and the grain sizes are even and uniform, thereby meeting related technical requirements of the sputtering target; and as a result, the high-purity titanium plate can be widely applied to the field of sputtering films of electronic devices, semiconductors, plane display and the like.
Description
Technical field
The invention belongs to Rare Metals Materials preparing technical field, be specifically related to a kind of preparation method of target high purity titanium plate.
Background technology
Target, as a kind of material with special purpose, has very strong application purpose and clear and definite application background.Sputtering target material has been widely used in the various fields such as decoration, tool and mould, glass, electron device, semi-conductor, magnetic recording, plane display, solar cell.Sputtering target material is a newer industry in China; Also there is larger gap in China's target technical industry level compared with international target, global high-end target market also mainly monopolize by American-European or Japanese target company.Up to now, China does not also produce the professional major company of target, and a large amount of target also need from external import, target particularly with high content of technology.
Pure titanium sputtering target has been widely used in the fields such as decoration film coating, tool and mould plated film, glass coating, semiconductor device plated film, electron device plated film, plane display plated film now.The production major control purity of target Titanium board, grain-size, grain orientation and grain uniformity four aspects.The field target purity requirement such as semiconductor device, electron device, plane display is high, requires that the quality purity of titanium plate reaches more than 99.8%.The purity of target is higher, and the performance of sputtered film is better; And the grain-size of target must control below 100 μm.In suitable grain size range, grain orientation is more evenly better; The target that grain-size difference is less, the thickness distribution of deposition film is also more even.Because target high purity titanium plate technique requires high, production difficulty is large, particularly the high-end target market such as electron device, semi-conductor, plane display, domestic specialized company and the mature technology also not producing target high purity titanium plate.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of target high purity titanium plate.The quality purity of the target high purity titanium plate adopting the method to prepare is not less than 99.8%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is less than 100 μm, even grain size is consistent, meet the associated specifications of high-end sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of target high purity titanium plate, and it is characterized in that, the method comprises the following steps:
Step one, titanium sponge particles is pressed into density is 3.2g/cm
3~ 3.5g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 480mm ~ 720mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, remove the surface imperfection of ingot casting, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 60min ~ 90min under the condition of 750 DEG C ~ 800 DEG C in temperature, be incubated 300min ~ 450min after being then warming up to 1000 DEG C ~ 1050 DEG C;
Step 4, the upsetting pull adopting quick forging machine the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 120mm ~ 240mm; The total deformation of described upsetting pull forging is 65% ~ 80%;
The surface imperfection of slab described in step 5, removal step four, then the slab after removal surface imperfection being placed in process furnace, is be incubated 150min ~ 280min under the condition of 850 DEG C ~ 880 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is rolled by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 10mm ~ 20mm; The total deformation of described rolling is 85% ~ 95%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 10mm ~ 20mm; The quality purity of described target high purity titanium plate is not less than 99.8%.
The preparation method of above-mentioned a kind of target high purity titanium plate, is characterized in that, the quality grade of titanium sponge particles described in step one is zero level.
The preparation method of above-mentioned a kind of target high purity titanium plate, is characterized in that, the granularity of titanium sponge particles described in step one is 0.83mm ~ 12.7mm.
The preparation method of above-mentioned a kind of target high purity titanium plate, is characterized in that, the speed heated up described in step 3 is 1 DEG C/and min ~ 2 DEG C/min
The preparation method of above-mentioned a kind of target high purity titanium plate, is characterized in that, the pass deformation of rolling described in step 6 is 8.5% ~ 30%.
The preparation method of above-mentioned a kind of target high purity titanium plate, is characterized in that, the temperature of annealing described in step 7 650 DEG C ~ 750 DEG C, and the time of described annealing is 30min ~ 60min.
The present invention compared with prior art has the following advantages:
1, first titanium sponge particles is obtained ingot casting through vacuum consumable arc-melting process by the present invention, then ingot casting is forged into slab, then slab rolling is become semifinished sheet, finally by annealing, aligning and figuring of surface process, finally obtains target high purity titanium plate; The present invention, by melting, forging, rolling and the optimization of annealing process procedure and the screening of processing parameter, finally makes the quality purity of target high purity titanium plate be not less than 99.8%; Wherein, in smelt stage, the present invention, by the density of control electrode block and the vacuum tightness of melting, makes the shrinkage cavity defect in melting greatly reduce, effectively can control the concentration of the interstitial elements such as oxygen, nitrogen, carbon, finally make ingot quality obtain strong guarantee; In the forging stage, first the present invention removes the surface imperfection of ingot casting, with the hole removing surface contamination layer and produce because of cold shut, prevents from surface imperfection to be brought into interiors of products through forging; Then the ingot casting removing surface imperfection is forged with aximal deformation value, make crystal grain obtain abundant fragmentation; At rolling sequence, slab is rolled with aximal deformation value by the present invention, makes that crystal grain obtains fully, homogeneous deformation.
2, the present invention adopts zero level titanium sponge to be raw material, and controls the granularity of titanium sponge, and raw-material purity can be made to be fully guaranteed, for the purity of target titanium plate provides powerful guarantee.
3, ingot casting is carried out the first heat treated by the present invention before forging, and adopts two benches heating cycle, first in 750 DEG C ~ 800 DEG C temperature ranges, carries out preheating 60min ~ 90min, and then is warming up to forging temperature 1000 DEG C ~ 1050 DEG C and heats; Two benches heating cycle can reduce inside ingot and the temperature contrast on surface greatly, effectively prevents the mass defect because internal and external temperature inequality causes.
The quality purity of the target high purity titanium plate 4, adopting the present invention to prepare is not less than 99.8%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is less than 100 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of target high purity titanium plate of the present invention.
Fig. 2 is the metallographic structure photo of target high purity titanium plate prepared by the embodiment of the present invention 1.
Embodiment
Embodiment 1
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.3g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; Can adopt the method for stirring that the size particles of zero level titanium sponge is uniformly distributed before compacting, to ensure the consistent in density of electrode block; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 560mm;
At the bottom of step 3, the rising head adopting the method for turning to excise ingot casting described in step 2 and ingot, the method stripped off the skin is adopted to remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 80min under the condition of 780 DEG C in temperature, be incubated 350min after being then warming up to 1050 DEG C with the temperature rise rate of 2 DEG C/min;
Step 4, the upsetting pull adopting quick forging machine the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 180mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 75%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 220min under the condition of 880 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 12 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 14mm; The total deformation of described rolling is 92.22%; The pass reduction of described rolling is respectively: 10.00%, 10.49%, 11.03%, 11.63%, 14.04%, 20.41%, 23.08%, 26.67%, 27.27%, 25.00%, 25.00% and 22.22%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 14mm; The temperature of described annealing is 680 DEG C, and the time of described annealing is 50min.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.9%, and the roughness of target high purity titanium plate is less than 2mm/m; The present embodiment target with the metallographic structure photo of high purity titanium plate as shown in Figure 1, the average grain size of the present embodiment target high purity titanium plate is 70 μm as seen from the figure, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Embodiment 2
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.4g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; Can adopt the method for stirring that the size particles of zero level titanium sponge is uniformly distributed before compacting, to ensure the consistent in density of electrode block; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 630mm;
At the bottom of step 3, the rising head adopting the method for turning to excise ingot casting described in step 2 and ingot, the method stripped off the skin is adopted to remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 90min under the condition of 760 DEG C in temperature, be incubated 400min after being then warming up to 1000 DEG C with the temperature rise rate of 2 DEG C/min;
Step 4, the upsetting pull adopting quick forging machine the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 220mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 73%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 260min under the condition of 880 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 14 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 18mm; The total deformation of described rolling is 91.82%; The pass reduction of described rolling is respectively: 8.64%, 9.45%, 9.34%, 9.09%, 11.33%, 15.79%, 16.96%, 18.28%, 19.74%, 21.31%, 20.83%, 21.05%, 23.33% and 21.74%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 18mm; The temperature of described annealing is 700 DEG C, and the time of described annealing is 40min.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.9%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is 65 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Embodiment 3
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.5g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; Can adopt the method for stirring that the size particles of zero level titanium sponge is uniformly distributed before compacting, to ensure the consistent in density of electrode block; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 720mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, and remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified with lathe by the method for turning, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 90min under the condition of 780 DEG C in temperature, be incubated 450min after being then warming up to 1020 DEG C with the temperature rise rate of 2 DEG C/min;
Step 4, the upsetting pull adopting forge press the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 240mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 80%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 280min under the condition of 860 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 13 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 20mm; The total deformation of described rolling is 91.67%, and pass reduction is respectively: 8.50%, 8.92%, 10.00%, 11.11%, 15.94%, 19.52%, 23.69%, 25.86%, 30.00%, 27.52%, 20.12%, 10.11% and 10.35%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 20mm; The temperature of described annealing is 650 DEG C, and the time of described annealing is 60min.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.95%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is 74 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Embodiment 4
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.2g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; Can adopt the method for stirring that the size particles of zero level titanium sponge is uniformly distributed before compacting, to ensure the consistent in density of electrode block; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 480mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, and remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified with lathe by the method for turning, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 80min under the condition of 750 DEG C in temperature, be incubated 300min after being then warming up to 1020 DEG C with the temperature rise rate of 2 DEG C/min;
Step 4, the upsetting pull adopting forge press the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 160mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 70%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 200min under the condition of 860 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 16 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 10mm; The total deformation of described rolling is 93.75%; The pass reduction of described rolling is respectively: 9.04%, and 9.54%, 10.00%, 10.32%, 10.97%, 12.85%, 15.87%, 20.64%, 24.79%, 26.68%, 27.98%, 18.55%, 15.32%, 14.88%, 13.52%, 9.25%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 10mm; The temperature of described annealing is 750 DEG C, and the time of described annealing is 30min.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.8%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is 80 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Embodiment 5
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.5g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; Can adopt the method for stirring that the size particles of zero level titanium sponge is uniformly distributed before compacting, to ensure the consistent in density of electrode block; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 560mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, and remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified with lathe by the method for turning, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 80min under the condition of 770 DEG C in temperature, be incubated 350min after being then warming up to 1020 DEG C with the temperature rise rate of 2 DEG C/min;
Step 4, the upsetting pull adopting forge press the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 240mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 65%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 270min under the condition of 860 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 14 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 12mm; The total deformation of described rolling is 95%; The pass reduction of described rolling is respectively: 10.00%, 11.23%, 12.31%, 12.38%, 14.66%, 15.34%, 15.86%, 20.64%, 24.79%, 28.94%, 30.00%, 27.66%, 21.55% and 20.47%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 12mm; The temperature of described annealing is 750 DEG C, and the time of described annealing is 30min.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.94%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is 60 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Embodiment 6
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.5g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; The method stirred is adopted the size particles of zero level titanium sponge to be uniformly distributed, to ensure the consistent in density of electrode block before compacting; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 630mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, and remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified with lathe by the method for turning, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 80min under the condition of 770 DEG C in temperature, be incubated 400min after being then warming up to 1020 DEG C with the temperature rise rate of 2 DEG C/min;
Step 4, the upsetting pull adopting forge press the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 200mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 78%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 240min under the condition of 860 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 14 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 18mm; The total deformation of described rolling is 91%; The pass reduction of described rolling is respectively: 8.50%, 8.87%, 9.06%, 9.99%, 10.88%, 14.63%, 15.96%, 20.97%, 25.87%, 27.54%, 20.10%, 18.63%, 15.61% and 11.45%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 18mm; The temperature of described annealing is 690 DEG C, and the time of described annealing is 45min; The quality purity of described target high purity titanium plate is not less than 99.8%.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.88%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is 73 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
Embodiment 7
Composition graphs 1, the preparation method of the present embodiment target high purity titanium plate comprises the following steps:
Step one, be 0.83mm ~ 12.7mm by granularity, and the zero level titanium sponge particles press meeting standard GB/T/T2524-2002 is pressed into density is 3.4g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode; Can adopt the method for stirring that the size particles of zero level titanium sponge is uniformly distributed before compacting, to ensure the consistent in density of electrode block; The electrode block suppressed need keep complete, without falling the defects such as slag, layering, crackle;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 480mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, and remove the surface imperfection of ingot casting until UT (Ultrasonic Testing) detection is qualified with lathe by the method for turning, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 60min under the condition of 800 DEG C in temperature, be incubated 380min after being then warming up to 1020 DEG C with the temperature rise rate of 1 DEG C/min;
Step 4, the upsetting pull adopting forge press the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 120mm; Described upsetting pull forging adopts first axial jumping-up, more axially pulling is to the forging mode of flat side, and the total deformation of described upsetting pull forging is 78%;
Described in the method removal step four of step 5, employing turnning and milling, the surface imperfection of slab is until UT (Ultrasonic Testing) detection is qualified, then the slab after removal surface imperfection being placed in process furnace, is be incubated 150min under the condition of 850 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is carried out 11 passes by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 18mm; The total deformation of described rolling is 85%; The pass reduction of described rolling is respectively: 8.5%, 10.32%, 11.25%, 15.66%, 18.12%, 20.44%, 22.30%, 25.78%, 20.54%, 10.52% and 8.50%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 18mm; The temperature of described annealing is 750 DEG C, and the time of described annealing is 30min.
The quality purity of target high purity titanium plate prepared by the present embodiment is 99.86%, the roughness of target high purity titanium plate is less than 2mm/m, the average grain size of target high purity titanium plate is 80 μm, even grain size is consistent, meet the associated specifications of sputtering target material, the sputtered film fields such as electron device, semi-conductor, plane display can be widely used in.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (3)
1. a target preparation method for high purity titanium plate, it is characterized in that, the method comprises the following steps:
Step one, titanium sponge particles is pressed into density is 3.2g/cm
3~ 3.5g/cm
3electrode block, then multiple described electrode block is carried out vacuum plasma welding in vacuum plasma welding box, obtains consumable electrode;
Step 2, consumable electrode described in step one is placed in vacuum consumable arc-melting stove, carries out twice vacuum consumable arc-melting be not more than the condition of 0.5Pa in vacuum tightness under, obtain ingot casting; The circle of the cross-sectional shape of described ingot casting to be diameter be 480mm ~ 720mm;
At the bottom of step 3, the rising head excising ingot casting described in step 2 and ingot, remove the surface imperfection of ingot casting, then the ingot casting after removal surface imperfection is placed in process furnace and carries out the first heat treated, the concrete system of described first heat treated is: be first be incubated 60min ~ 90min under the condition of 750 DEG C ~ 800 DEG C in temperature, be incubated 300min ~ 450min after being then warming up to 1000 DEG C ~ 1050 DEG C;
Step 4, the upsetting pull adopting quick forging machine the ingot casting in step 3 after the first heat treated to be carried out a fire secondary are forged, and obtain the slab that thickness is 120mm ~ 240mm; The total deformation of described upsetting pull forging is 65% ~ 80%;
The surface imperfection of slab described in step 5, removal step four, then the slab after removal surface imperfection being placed in process furnace, is be incubated 150min ~ 280min under the condition of 850 DEG C ~ 880 DEG C to carry out the second heat treated in temperature;
Slab in step 5 after the second heat treated is rolled by step 6, employing hot rolls, obtains the semifinished sheet that thickness is 10mm ~ 20mm; The total deformation of described rolling is 85% ~ 95%;
Step 7, semifinished sheet described in step 6 is carried out annealing, aligning and figuring of surface process successively, obtain the target high purity titanium plate that thickness is 10mm ~ 20mm; The quality purity of described target high purity titanium plate is not less than 99.8%; The temperature of described annealing 650 DEG C ~ 750 DEG C, the time of described annealing is 30min ~ 60min;
The granularity of titanium sponge particles described in step one is 0.83mm ~ 12.7mm; The quality grade of titanium sponge particles described in step one is zero level.
2. the preparation method of a kind of target high purity titanium plate according to claim 1, is characterized in that, the speed heated up described in step 3 is 1 DEG C/and min ~ 2 DEG C/min.
3. the preparation method of a kind of target high purity titanium plate according to claim 1, is characterized in that, the pass deformation of rolling described in step 6 is 8.5% ~ 30%.
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| CN106346199B (en) * | 2016-08-31 | 2018-07-10 | 宝鸡市永盛泰钛业有限公司 | The manufacturing method of backplate under a kind of titanium alloy car floor |
| CN106881564A (en) * | 2017-01-09 | 2017-06-23 | 洛阳双瑞精铸钛业有限公司 | A kind of method that utilization thin-walled major diameter titanium welding pipe produces titanium matter cup/kettle |
| CN107916352A (en) * | 2017-11-17 | 2018-04-17 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for manufacturing jewellery |
| CN111687233A (en) * | 2019-03-15 | 2020-09-22 | 宝鸡聚和信钛业有限公司 | Production method of pure titanium plate blank |
| CN111304463A (en) * | 2020-03-13 | 2020-06-19 | 中铝沈阳有色金属加工有限公司 | Vacuum consumable melting method of high-purity titanium cast ingot |
| CN113106362B (en) * | 2021-03-18 | 2022-07-01 | 先导薄膜材料（广东）有限公司 | Manufacturing method of target material back plate with concave surface |
| CN114393055A (en) * | 2021-12-14 | 2022-04-26 | 新疆湘润新材料科技有限公司 | Preparation method of titanium strip coil for composite vacuum cup |
| CN114717528B (en) * | 2022-04-06 | 2023-09-08 | 宁波江丰电子材料股份有限公司 | Titanium-containing target material and preparation method thereof |
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