CN103215553A - 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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- CN103215553A CN103215553A CN2013101524283A CN201310152428A CN103215553A CN 103215553 A CN103215553 A CN 103215553A CN 2013101524283 A CN2013101524283 A CN 2013101524283A CN 201310152428 A CN201310152428 A CN 201310152428A CN 103215553 A CN103215553 A CN 103215553A
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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 the Rare Metals Materials preparing technical field, be specifically related to the preparation method of a kind of target with the high purity titanium plate.
Background technology
Target has very strong application purpose and definite application background as a kind of material with special purpose.Sputtering target material has been widely used in various fields such as decoration, tool and mould, glass, electron device, semi-conductor, magnetic recording, plane demonstration, solar cell.Sputtering target material is a newer industry in China; China's target technical industry level is compared the also bigger gap of existence with international target, global high-end target market is also mainly monopolized by American-European or Japanese target company.Up to now, the professional major company that China does not also produce target, a large amount of targets also need from external import, target particularly with high content of technology.
Pure titanium sputtering target has been widely used in fields such as decoration film coating, tool and mould plated film, glass coating, semiconductor device plated film, electron device plated film, plane demonstration plated film now.Target is with production major control purity, grain-size, grain orientation and four aspects of uniform crystal particles of pure titanium plate.Fields such as semiconductor device, electron device, plane demonstration require the quality purity of titanium plate to reach more than 99.8% with target purity requirement height.The purity of target is high more, and the performance of sputtered film is good more; And the grain-size of target must be controlled at below the 100 μ m.In suitable grain size range, grain orientation is even more good more; Grain-size differs less target, and the thickness distribution of deposition film is also more even.Because it is high that target requires with the high purity titanium plate technique, the production difficulty is big, high-end target markets such as electron device, semi-conductor, plane demonstration particularly, domestic specialized company and the mature technology of also not producing target with the high purity titanium plate.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned the deficiencies in the prior art, and the preparation method of a kind of target with the high purity titanium plate is provided.The target that adopts the preparation of this method is not less than 99.8% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target uses the average grain size of high purity titanium plate less than 100 μ m, the even grain size unanimity, satisfy the correlation technique requirement of high-end sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of target preparation method of high purity titanium plate is characterized in that this method may further comprise the steps:
Step 1, the titanium sponge particle is pressed into density is 3.2g/cm
3～3.5g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 480mm～720mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, remove the surface imperfection of ingot casting, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 60min～90min under temperature is 750 ℃～800 ℃ condition, be incubated 300min～450min after being warming up to 1000 ℃～1050 ℃ then;
Step 4, the fast forging machine of employing carry out the inferior upsetting pull of a fire with the ingot casting after first heat treated in the step 3 and forge, and obtain the slab that thickness is 120mm～240mm; The forged total deformation of described upsetting pull is 65%～80%;
Step 5, remove the surface imperfection of slab described in the step 4, the slab that will remove then after the surface imperfection places process furnace, in temperature is to be incubated 150min～280min under 850 ℃～880 ℃ the condition to carry out second heat treated;
Step 6, employing hot rolls are rolled the slab after second heat treated in the step 5, obtain the semifinished sheet that thickness is 10mm～20mm; Described rolling total deformation is 85%～95%;
Step 7, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 10mm～20mm; Described target is not less than 99.8% with the quality purity of high purity titanium plate.
Above-mentioned a kind of target is characterized in that with the preparation method of high purity titanium plate the particulate of titanium sponge described in step 1 quality grade is a zero level.
Above-mentioned a kind of target is characterized in that with the preparation method of high purity titanium plate the particulate of titanium sponge described in step 1 granularity is 0.83mm～12.7mm.
Above-mentioned a kind of target is characterized in that with the preparation method of high purity titanium plate, and the speed that heats up described in the step 3 is 1 ℃/min～2 ℃/min
Above-mentioned a kind of target is characterized in that with the preparation method of high purity titanium plate rolling pass deformation is 8.5%～30% described in the step 6.
Above-mentioned a kind of target is characterized in that with the preparation method of high purity titanium plate, 650 ℃～750 ℃ of the temperature of annealed described in the step 7, and the described annealed time is 30min～60min.
The present invention compared with prior art has the following advantages:
1, the present invention at first handles the titanium sponge particle and obtains ingot casting through vacuum consumable arc-melting, again ingot casting is forged into slab, then slab rolling is become semifinished sheet, after annealing, aligning and figuring of surface are handled, finally obtains target high purity titanium plate; The present invention finally makes target be not less than 99.8% with the quality purity of high purity titanium plate by to melting, forging, rolling and the optimization of annealing process procedure and the screening of processing parameter; Wherein, in smelt stage, the present invention reduces the shrinkage cavity defect in the melting by the density of control electrode piece and the vacuum tightness of melting greatly, can effectively control the concentration of interstitial elements such as oxygen, nitrogen, carbon, finally makes ingot quality obtain strong guarantee; In the forging stage, the present invention at first removes the surface imperfection of ingot casting, to remove surface contamination layer and because of the hole that cold shut was produced, to prevent from surface imperfection is brought into product inside through forging; The ingot casting that to remove surface imperfection forges with aximal deformation value then, makes crystal grain obtain abundant fragmentation; At rolling sequence, the present invention is rolled slab with aximal deformation value, makes that crystal grain obtains fully, homogeneous deformation.
2, to adopt the zero level titanium sponge be raw material in the present invention, and the granularity of titanium sponge is controlled, and purity of raw materials is fully guaranteed, for target provides powerful guarantee with the purity of titanium plate.
3, the present invention carries out first heat treated with ingot casting before forging, and adopts two stage heating cycles, at first carries out preheating 60min～90min in 750 ℃～800 ℃ temperature ranges, and then is warming up to forging temperature and heats for 1000 ℃～1050 ℃; Two stage heating cycles can reduce inner with the surperficial temperature contrast of ingot casting greatly, effectively prevent because the mass defect that the internal and external temperature inequality is caused.
4, the target of employing the present invention preparation is not less than 99.8% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target uses the average grain size of high purity titanium plate less than 100 μ m, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Below in conjunction with drawings and Examples the present invention is described in further detail.
Description of drawings
Fig. 1 is the preparation technology schema of target of the present invention with the high purity titanium plate.
Fig. 2 is the metallographic structure photo of the target of the embodiment of the invention 1 preparation with the high purity titanium plate.
Embodiment
Embodiment 1
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.3g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; Can adopt stirring method to make the size particles uniform distribution of zero level titanium sponge before the compacting, with the consistent in density of assurance electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 560mm;
The method of step 3, employing turning is excised at the bottom of the rising head and ingot of ingot casting described in the step 2, the surface imperfection that the method that employing strips off the skin is removed ingot casting is qualified until the UT (Ultrasonic Testing) detection, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 80min under temperature is 780 ℃ condition, be incubated 350min after being warming up to 1050 ℃ with the temperature rise rate of 2 ℃/min then;
Step 4, the fast forging machine of employing carry out the inferior upsetting pull of a fire with the ingot casting after first heat treated in the step 3 and forge, and obtain the slab that thickness is 180mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 75%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 220min carries out second heat treated under 880 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 12 passages rolling, obtains the semifinished sheet that thickness is 14mm; Described rolling total deformation is 92.22%; Described rolling pass reduction 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 14mm; Described annealed temperature is 680 ℃, and the described annealed time is 50min.
The target of present embodiment preparation is 99.9% with the quality purity of high purity titanium plate, and target uses the roughness of high purity titanium plate less than 2mm/m; The metallographic structure photo of present embodiment target usefulness high purity titanium plate as shown in Figure 1, the present embodiment target is 70 μ m with the average grain size of high purity titanium plate as seen from the figure, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Embodiment 2
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.4g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; Can adopt stirring method to make the size particles uniform distribution of zero level titanium sponge before the compacting, with the consistent in density of assurance electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 630mm;
The method of step 3, employing turning is excised at the bottom of the rising head and ingot of ingot casting described in the step 2, the surface imperfection that the method that employing strips off the skin is removed ingot casting is qualified until the UT (Ultrasonic Testing) detection, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 90min under temperature is 760 ℃ condition, be incubated 400min after being warming up to 1000 ℃ with the temperature rise rate of 2 ℃/min then;
Step 4, the fast forging machine of employing carry out the inferior upsetting pull of a fire with the ingot casting after first heat treated in the step 3 and forge, and obtain the slab that thickness is 220mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 73%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 260min carries out second heat treated under 880 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 14 passages rolling, obtains the semifinished sheet that thickness is 18mm; Described rolling total deformation is 91.82%; Described rolling pass reduction 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 18mm; Described annealed temperature is 700 ℃, and the described annealed time is 40min.
The target of present embodiment preparation is 99.9% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target is 65 μ m with the average grain size of high purity titanium plate, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Embodiment 3
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.5g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; Can adopt stirring method to make the size particles uniform distribution of zero level titanium sponge before the compacting, with the consistent in density of assurance electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 720mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, and it is qualified by the surface imperfection of the method removal ingot casting of turning until the UT (Ultrasonic Testing) detection with lathe, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 90min under temperature is 780 ℃ condition, be incubated 450min after being warming up to 1020 ℃ with the temperature rise rate of 2 ℃/min then;
Step 4, employing oil pressure are forged machine soon the ingot casting after first heat treated in the step 3 are carried out the inferior upsetting pull forging of a fire, obtain the slab that thickness is 240mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 80%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 280min carries out second heat treated under 860 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 13 passages rolling, obtains the semifinished sheet that thickness is 20mm; Described rolling total deformation 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 20mm; Described annealed temperature is 650 ℃, and the described annealed time is 60min.
The target of present embodiment preparation is 99.95% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target is 74 μ m with the average grain size of high purity titanium plate, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Embodiment 4
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.2g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; Can adopt stirring method to make the size particles uniform distribution of zero level titanium sponge before the compacting, with the consistent in density of assurance electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 480mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, and it is qualified by the surface imperfection of the method removal ingot casting of turning until the UT (Ultrasonic Testing) detection with lathe, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 80min under temperature is 750 ℃ condition, be incubated 300min after being warming up to 1020 ℃ with the temperature rise rate of 2 ℃/min then;
Step 4, employing oil pressure are forged machine soon the ingot casting after first heat treated in the step 3 are carried out the inferior upsetting pull forging of a fire, obtain the slab that thickness is 160mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 70%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 200min carries out second heat treated under 860 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 16 passages rolling, obtains the semifinished sheet that thickness is 10mm; Described rolling total deformation is 93.75%; Described rolling pass reduction is respectively: 9.04%, 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 10mm; Described annealed temperature is 750 ℃, and the described annealed time is 30min.
The target of present embodiment preparation is 99.8% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target is 80 μ m with the average grain size of high purity titanium plate, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Embodiment 5
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.5g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; Can adopt stirring method to make the size particles uniform distribution of zero level titanium sponge before the compacting, with the consistent in density of assurance electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 560mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, and it is qualified by the surface imperfection of the method removal ingot casting of turning until the UT (Ultrasonic Testing) detection with lathe, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 80min under temperature is 770 ℃ condition, be incubated 350min after being warming up to 1020 ℃ with the temperature rise rate of 2 ℃/min then;
Step 4, employing oil pressure are forged machine soon the ingot casting after first heat treated in the step 3 are carried out the inferior upsetting pull forging of a fire, obtain the slab that thickness is 240mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 65%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 270min carries out second heat treated under 860 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 14 passages rolling, obtains the semifinished sheet that thickness is 12mm; Described rolling total deformation is 95%; Described rolling pass reduction 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 12mm; Described annealed temperature is 750 ℃, and the described annealed time is 30min.
The target of present embodiment preparation is 99.94% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target is 60 μ m with the average grain size of high purity titanium plate, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Embodiment 6
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.5g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; The employing stirring method makes the size particles uniform distribution of zero level titanium sponge before the compacting, to guarantee the consistent in density of electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 630mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, and it is qualified by the surface imperfection of the method removal ingot casting of turning until the UT (Ultrasonic Testing) detection with lathe, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 80min under temperature is 770 ℃ condition, be incubated 400min after being warming up to 1020 ℃ with the temperature rise rate of 2 ℃/min then;
Step 4, employing oil pressure are forged machine soon the ingot casting after first heat treated in the step 3 are carried out the inferior upsetting pull forging of a fire, obtain the slab that thickness is 200mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 78%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 240min carries out second heat treated under 860 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 14 passages rolling, obtains the semifinished sheet that thickness is 18mm; Described rolling total deformation is 91%; Described rolling pass reduction 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 18mm; Described annealed temperature is 690 ℃, and the described annealed time is 45min; Described target is not less than 99.8% with the quality purity of high purity titanium plate.
The target of present embodiment preparation is 99.88% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target is 73 μ m with the average grain size of high purity titanium plate, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
Embodiment 7
In conjunction with Fig. 1, the present embodiment target may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, be 0.83mm～12.7mm with granularity, and the zero level titanium sponge particle that satisfies standard GB/T2524-2002 to be pressed into density with press be 3.4g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode; Can adopt stirring method to make the size particles uniform distribution of zero level titanium sponge before the compacting, with the consistent in density of assurance electrode block; The electrode block that compacting is finished need be kept perfectly, and does not have the defectives such as slag, layering, crackle of falling;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 480mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, and it is qualified by the surface imperfection of the method removal ingot casting of turning until the UT (Ultrasonic Testing) detection with lathe, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 60min under temperature is 800 ℃ condition, be incubated 380min after being warming up to 1020 ℃ with the temperature rise rate of 1 ℃/min then;
Step 4, employing oil pressure are forged machine soon the ingot casting after first heat treated in the step 3 are carried out the inferior upsetting pull forging of a fire, obtain the slab that thickness is 120mm; Described upsetting pull is forged and is adopted earlier axially jumping-up, and axially pulling is to flat side's forging mode again, and the forged total deformation of described upsetting pull is 78%;
The surface imperfection that the method for step 5, employing turnning and milling is removed slab described in the step 4 is qualified until the UT (Ultrasonic Testing) detection, the slab that to remove then after the surface imperfection places process furnace, is that insulation 150min carries out second heat treated under 850 ℃ the condition in temperature;
Step 6, to adopt hot rolls that the slab after second heat treated in the step 5 is carried out 11 passages rolling, obtains the semifinished sheet that thickness is 18mm; Described rolling total deformation is 85%; Described rolling pass reduction 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, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 18mm; Described annealed temperature is 750 ℃, and the described annealed time is 30min.
The target of present embodiment preparation is 99.86% with the quality purity of high purity titanium plate, target uses the roughness of high purity titanium plate less than 2mm/m, target is 80 μ m with the average grain size of high purity titanium plate, the even grain size unanimity, satisfy the correlation technique requirement of sputtering target material, can be widely used in sputtered film fields such as electron device, semi-conductor, plane demonstration.
The above only is preferred embodiment of the present invention, is not that the present invention is imposed any restrictions.Everyly any simple modification that above embodiment did, change and equivalence are changed, all still belong in the protection domain of technical solution of the present invention according to the invention technical spirit.
Claims (6)
1. a target is characterized in that this method may further comprise the steps with the preparation method of high purity titanium plate:
Step 1, the titanium sponge particle is pressed into density is 3.2g/cm
3～3.5g/cm
3Electrode block, then a plurality of described electrode blocks are carried out the vacuum plasma welding in vacuum plasma weldering case, obtain consumable electrode;
Step 2, consumable electrode described in the step 1 is placed the vacuum consumable arc-melting stove, be not more than in vacuum tightness under the condition of 0.5Pa and carry out vacuum consumable arc-melting twice, obtain ingot casting; The cross-sectional shape of described ingot casting is that diameter is the circle of 480mm～720mm;
Described in step 3, the excision step 2 at the bottom of the rising head and ingot of ingot casting, remove the surface imperfection of ingot casting, the ingot casting that to remove then after the surface imperfection places process furnace to carry out first heat treated, the concrete system of described first heat treated is: at first be incubated 60min～90min under temperature is 750 ℃～800 ℃ condition, be incubated 300min～450min after being warming up to 1000 ℃～1050 ℃ then;
Step 4, the fast forging machine of employing carry out the inferior upsetting pull of a fire with the ingot casting after first heat treated in the step 3 and forge, and obtain the slab that thickness is 120mm～240mm; The forged total deformation of described upsetting pull is 65%～80%;
Step 5, remove the surface imperfection of slab described in the step 4, the slab that will remove then after the surface imperfection places process furnace, in temperature is to be incubated 150min～280min under 850 ℃～880 ℃ the condition to carry out second heat treated;
Step 6, employing hot rolls are rolled the slab after second heat treated in the step 5, obtain the semifinished sheet that thickness is 10mm～20mm; Described rolling total deformation is 85%～95%;
Step 7, with semifinished sheet described in the step 6 anneal successively, aligning and figuring of surface handle, obtaining thickness is the target high purity titanium plate of 10mm～20mm; Described target is not less than 99.8% with the quality purity of high purity titanium plate.
2. a kind of target according to claim 1 is characterized in that with the preparation method of high purity titanium plate the particulate of titanium sponge described in step 1 quality grade is a zero level.
3. a kind of target according to claim 1 is characterized in that with the preparation method of high purity titanium plate the particulate of titanium sponge described in step 1 granularity is 0.83mm～12.7mm.
4. a kind of target according to claim 1 is characterized in that with the preparation method of high purity titanium plate, and the speed that heats up described in the step 3 is 1 ℃/min～2 ℃/min.
5. a kind of target according to claim 1 is characterized in that with the preparation method of high purity titanium plate rolling pass deformation is 8.5%～30% described in the step 6.
6. a kind of target according to claim 1 is characterized in that with the preparation method of high purity titanium plate, 650 ℃～750 ℃ of the temperature of annealed described in the step 7, and the described annealed time is 30min～60min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106346199A (en) * | 2016-08-31 | 2017-01-25 | 宝鸡市永盛泰钛业有限公司 | Method for manufacturing titanium alloy lower protective plate of automobile bottom plate |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08232061A (en) * | 1995-02-27 | 1996-09-10 | Sumitomo Sitix Corp | Method for forging high purity titanium material |
| US20030132108A1 (en) * | 2002-01-15 | 2003-07-17 | Shoichi Takahashi | Process for producing titanium material for target, titanium material for target, and sputtering target using the same |
| CN101906602A (en) * | 2010-09-10 | 2010-12-08 | 攀钢集团钢铁钒钛股份有限公司 | Method for processing metastable beta-type titanium alloy plate |
| CN102151774A (en) * | 2011-03-16 | 2011-08-17 | 湖南金天钛业科技有限公司 | Production method of large-size high-unit-weight pure-titanium forging plate blank |
| CN102453873A (en) * | 2010-10-26 | 2012-05-16 | 宝鸡市嘉诚稀有金属材料有限公司 | Titanium target material and manufacturing method thereof |
| CN103008978A (en) * | 2011-09-21 | 2013-04-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium plate billet |
-
2013
- 2013-04-27 CN CN201310152428.3A patent/CN103215553B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08232061A (en) * | 1995-02-27 | 1996-09-10 | Sumitomo Sitix Corp | Method for forging high purity titanium material |
| US20030132108A1 (en) * | 2002-01-15 | 2003-07-17 | Shoichi Takahashi | Process for producing titanium material for target, titanium material for target, and sputtering target using the same |
| CN101906602A (en) * | 2010-09-10 | 2010-12-08 | 攀钢集团钢铁钒钛股份有限公司 | Method for processing metastable beta-type titanium alloy plate |
| CN102453873A (en) * | 2010-10-26 | 2012-05-16 | 宝鸡市嘉诚稀有金属材料有限公司 | Titanium target material and manufacturing method thereof |
| CN102151774A (en) * | 2011-03-16 | 2011-08-17 | 湖南金天钛业科技有限公司 | Production method of large-size high-unit-weight pure-titanium forging plate blank |
| CN103008978A (en) * | 2011-09-21 | 2013-04-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium plate billet |
Non-Patent Citations (1)
| Title |
|---|
| 谢成木: "《钛及钛合金铸造》", 31 December 2005, article "钛及钛合金铸造", pages: 279 - 411-412 * |
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| CN106346199A (en) * | 2016-08-31 | 2017-01-25 | 宝鸡市永盛泰钛业有限公司 | Method for manufacturing titanium alloy lower protective plate of automobile bottom plate |
| 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 |
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| 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 |
| CN113106362A (en) * | 2021-03-18 | 2021-07-13 | 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 |
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