CN104831245A - Hot isostatic pressing production method of tubular molybdenum alloy sputtering target - Google Patents
Hot isostatic pressing production method of tubular molybdenum alloy sputtering target Download PDFInfo
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- CN104831245A CN104831245A CN201510290578.XA CN201510290578A CN104831245A CN 104831245 A CN104831245 A CN 104831245A CN 201510290578 A CN201510290578 A CN 201510290578A CN 104831245 A CN104831245 A CN 104831245A
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Abstract
The invention provides a hot isostatic pressing production method of a tubular molybdenum alloy sputtering target. The method includes the steps of firstly, manufacturing a hot isostatic pressing sheath according to the design requirements of the to-be-produced tubular molybdenum alloy sputtering target; secondly, loading molybdenum alloy powder into the hot isostatic pressing sheath; thirdly, performing vacuum thermal processing; fourthly, nesting core material into the hot isostatic pressing sheath, performing hot isostatic pressing forming, removing the core material after cooling along with a furnace, and taking out the formed product from the hot isostatic pressing sheath to obtain the tubular molybdenum alloy sputtering target. The method has the advantages that the method is simple in production process and hardly limited in material categories and alloy components, and the produced target is high in compactness and low in impurity content.
Description
Technical field
The invention belongs to powder metallurgical technology, be specifically related to a kind of hot isostatic pressing preparation method of tubulose molybdenum alloy sputtering target.
Background technology
The tubulose molybdenum alloy sputtering target that utilization ratio is higher in recent years obtains the extensive investigation and application of external large-scale target manufacturers, its utilization ratio can reach 70% in theory, being much higher than the rate of utilization of planar target 20% ~ 30%, therefore reducing plated film production cost, is the direction of target development.
Tubulose molybdenum alloy sputtering target, as Mo-10Nb, Mo-20Nb, Mo-20Nb-1Zr, Mo-15Nb-5Ta etc., alloy content is high, and high-temperature brittleness is large, is difficult to carry out press working.Tungsten, chromium and alloy in addition, fragility is large, is difficult to carry out press working.
Current difficult work brittleness metal and compo pipe target thereof mainly adopt sintering process to prepare.It is on the low side that sintering process prepares pipe target density, generally only has about 95%, is difficult to accomplish full densification because its shape is elongated tubular, compression moulding process and sintering process yielding, yield rate is lower.Another kind method adopts plasma spraying method to prepare pipe target.Plasma spraying method adopts plasma spraying to prepare sputtering layer in the tube surfaces of stainless steel tube or other materials, can adopt the further densification of hot isostatic pressing.Plasma spray coating process suitable material scope is wide, but the sputtering layer foreign matter content of preparation is high, and compactness is poor, and cost is higher, high to equipment requirements, limits the use of this technique.
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 tubulose molybdenum alloy sputtering target.The method technique is simple, and material category and alloying constituent are restricted hardly, and made target density is high, and foreign matter content is low.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of hot isostatic pressing preparation method of tubulose molybdenum alloy sputtering target, and it is characterized in that, the method comprises the following steps:
Step one, require to make hot isostatic pressing jacket according to the shape and size of tubulose molybdenum alloy sputtering target to be prepared, described hot isostatic pressing jacket comprises the first pipe fitting and is sleeved on the second outer and coaxial with the first pipe fitting pipe fitting of the first pipe fitting, the lower end of described first pipe fitting is connected by the first annular plate with the lower end of the second pipe fitting, the upper end of described first pipe fitting is connected by the second annular plate with the upper end of the second pipe fitting, and described second annular plate offers opening for feed and bleeding point;
Step 2, molybdenum alloy powder is loaded in hot isostatic pressing jacket by opening for feed described in step one, sealing opening for feed after jolt ramming on shaking platform;
Step 3, will be equipped with in step 2 the hot isostatic pressing jacket of molybdenum alloy powder bleeding point connect vacuum pump, then put into retort furnace, be not more than 5 × 10 in vacuum tightness
-2pa, temperature is vacuum heat treatment 0.5h ~ 4h under the condition of 150 DEG C ~ 400 DEG C, sealing bleeding point after naturally cooling;
Step 4, be contained in core/sleeve in step 3 after vacuum heat treatment hot isostatic pressing jacket in, then hot isostatic pressing stove is put into, it is 800 DEG C ~ 1600 DEG C in temperature, pressure is hip moulding 2h ~ 6h under the condition of 150MPa ~ 200MPa, core is removed after furnace cooling, from hot isostatic pressing jacket, take out moulding product, obtain tubulose molybdenum alloy sputtering target.
The hot isostatic pressing preparation method of above-mentioned a kind of tubulose molybdenum alloy sputtering target, is characterized in that, the material of the first pipe fitting and the second pipe fitting described in step one is pure titanium or 20# steel.
The hot isostatic pressing preparation method of above-mentioned a kind of tubulose molybdenum alloy sputtering target, it is characterized in that, described in step one, the wall thickness of the first pipe fitting and the second pipe fitting is 1.5mm ~ 4mm.
The hot isostatic pressing preparation method of above-mentioned a kind of tubulose molybdenum alloy sputtering target, is characterized in that, the powder of molybdenum alloy described in step 2 is molybdenum niobium alloy powder, molybdenum niobium zirconium alloy powder or molybdenum niobium tantalum alloy powder.
The hot isostatic pressing preparation method of above-mentioned a kind of tubulose molybdenum alloy sputtering target, is characterized in that, the thick walled steel tube of to be wall thickness the be 10mm ~ 25mm of core described in step 4, the external diameter 0.5mm ~ 1mm less of the internal diameter of the first pipe fitting of described core.
The hot isostatic pressing preparation method of above-mentioned a kind of tubulose molybdenum alloy sputtering target, is characterized in that, core described in step 4 is cylindrical graphite bar, the diameter of section 0.5mm ~ 1mm less of the internal diameter of the first pipe fitting of described core.
The hot isostatic pressing preparation method of above-mentioned a kind of tubulose molybdenum alloy sputtering target, is characterized in that, the internal diameter of the molybdenum alloy sputtering target of tubulose described in step 4 is 40mm ~ 205mm, and the wall thickness of described tubulose molybdenum alloy sputtering target is 15mm ~ 30mm.
The present invention compared with prior art has the following advantages:
1, the present invention carries out vacuumizing process while heating molybdenum alloy powder, and can remove the oxygen in molybdenum alloy powder, then sealing bleeding point makes powder hole keep vacuum, improves material purity.
2, the present invention puts into core in hot isostatic pressing jacket, accurately can control the internal diameter size of jacket after hip moulding, and the planeness of length direction after controlling jacket and material inside hip moulding.
3, the present invention is suitable for preparing various difficulty of processing greatly, the molybdenum that high/low temperature fragility is large, tungsten, zirconium, chromium, niobium-base alloy, and the various alloy materials with similar feature.
4, the invention provides a kind of method preparing molybdenum alloy tubulose rotary sputtering target material, compared with common preparation method, the present invention can process various brittle alloy pipe target, and product density is up to more than 99.5%, material purity is high, and the integrated yield of material is high.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the structural representation of hot isostatic pressing jacket of the present invention.
Fig. 2 is the A-A sectional view of Fig. 1.
Description of reference numerals:
1-the first pipe fitting; 2-the second pipe fitting; 3-opening for feed;
4-bleeding point; 5-the first annular plate; 6-the second annular plate.
Embodiment
The structure that hot isostatic pressing of the present invention prepares the hot isostatic pressing jacket that tubulose molybdenum alloy sputtering target adopts is described by embodiment 1.
Embodiment 1
As depicted in figs. 1 and 2, the present embodiment hot isostatic pressing jacket comprises the first pipe fitting 1 and is sleeved on the second outer and coaxial with the first pipe fitting 1 pipe fitting 2 of the first pipe fitting 1, the lower end of described first pipe fitting 1 is connected by the first annular plate 5 with the lower end of the second pipe fitting 2, the upper end of described first pipe fitting 1 is connected by the second annular plate 6 with the upper end of the second pipe fitting 2, and described second annular plate 6 offers opening for feed 3 and bleeding point 4.The material of described first pipe fitting 1 and the second pipe fitting 2 is preferably pure titanium or 20# steel.The wall thickness of described first pipe fitting 1 and the second pipe fitting 2 is preferably 1.5mm ~ 4mm.
The method utilizing hot isostatic pressing jacket described in embodiment 1 to prepare tubulose molybdenum alloy sputtering target is described by embodiment 2 to embodiment 5.
Embodiment 2
Composition graphs 1 and Fig. 2, the hot isostatic pressing preparation method of the present embodiment tubulose molybdenum alloy sputtering target comprises the following steps:
Step one, make hot isostatic pressing jacket according to the design requirements of tubulose molybdenum alloy sputtering target to be prepared; The external diameter of the hot isostatic pressing jacket made by the present embodiment is 168mm, internal diameter is 120mm, length is 1950mm, wall thickness is 2mm, opening for feed 3 is the circular hole of diameter 20mm, and mouth 4 of finding time is the circular hole of diameter 8mm, can weld an internal diameter 8mm in actual mechanical process at bleeding point 4 place, the steel pipe of wall thickness 3mm, length 500mm is so that vacuum pumping;
Step 2, molybdenum alloy powder is loaded in hot isostatic pressing jacket by opening for feed 3 described in step one, sealing opening for feed 3 after jolt ramming on shaking platform; Described molybdenum alloy powder is preferably powdered alloy, and wherein Mo is 80wt%, Nb is 20wt%; After jolt ramming, the relative density of molybdenum alloy powder is 60%;
Step 3, the bleeding point 4 of the hot isostatic pressing jacket that molybdenum alloy powder is housed in step 2 is connected vacuum pump, then put into retort furnace, be not more than 5 × 10 in vacuum tightness
-2pa, temperature is vacuum heat treatment 1h under the condition of 300 DEG C, carries out sealing after naturally cooling to bleeding point 4;
The cylindrical graphite bar of step 4, selection diameter of section 1mm less of the internal diameter of the first pipe fitting 1 is core, core/sleeve is contained in the hot isostatic pressing jacket in step 3 after vacuum heat treatment, then hot isostatic pressing stove is put into, it is 1400 DEG C in temperature, pressure is hip moulding 3h under the condition of 195MPa, remove core after furnace cooling, from hot isostatic pressing jacket, take out moulding product, obtain tubulose molybdenum alloy sputtering target.
The internal diameter of tubulose molybdenum alloy sputtering target prepared by the present embodiment is 125mm, and wall thickness is 15mm, and length is 1610mm.After testing, the actual density of tubulose molybdenum alloy sputtering target that prepared by the present embodiment is 99.75% of theoretical density.After testing, oxygen level is 145ppm.It can thus be appreciated that the density of tubulose molybdenum alloy sputtering target prepared by the present embodiment is high, product purity is high, and foreign matter content is low.
Embodiment 3
Composition graphs 1 and Fig. 2, the hot isostatic pressing preparation method of the present embodiment tubulose molybdenum alloy sputtering target comprises the following steps:
Step one, make hot isostatic pressing jacket according to the design requirements of tubulose molybdenum alloy sputtering target to be prepared; The external diameter of the hot isostatic pressing jacket made by the present embodiment is 165mm, internal diameter is 110mm, length is 1900mm, wall thickness is 3mm, opening for feed 3 is the circular hole of diameter 25mm, and mouth 4 of finding time is the circular hole of diameter 6mm, can weld an internal diameter 6mm in actual mechanical process at bleeding point 4 place, the titanium pipe of wall thickness 2.5mm, length 600mm is so that vacuum pumping;
Step 2, molybdenum alloy powder is loaded in hot isostatic pressing jacket by opening for feed 3 described in step one, sealing opening for feed 3 after jolt ramming on shaking platform; Described molybdenum alloy powder is preferably molybdenum niobium zirconium alloy powder, and wherein Mo is 80wt%, Nb be 15wt%, Zr is 5wt%, and after jolt ramming, the relative density of molybdenum alloy powder is 42%;
Step 3, the bleeding point 4 of the hot isostatic pressing jacket that molybdenum alloy powder is housed in step 2 is connected vacuum pump, then put into retort furnace, be not more than 5 × 10 in vacuum tightness
-2pa, temperature is vacuum heat treatment 2h under the condition of 200 DEG C, carries out sealing after naturally cooling to bleeding point 4;
The cylindrical graphite bar of step 4, selection diameter of section 0.5mm less of the internal diameter of the first pipe fitting 1 is core, core/sleeve is contained in the hot isostatic pressing jacket in step 3 after vacuum heat treatment, then hot isostatic pressing stove is put into, it is 1500 DEG C in temperature, pressure is hip moulding 4h under the condition of 195MPa, remove core after furnace cooling, from hot isostatic pressing jacket, take out moulding product, obtain tubulose molybdenum alloy sputtering target.
The internal diameter of tubulose molybdenum alloy sputtering target prepared by the present embodiment is 118mm, and wall thickness is 15mm, and length is 1850mm.After testing, the actual density of tubulose molybdenum alloy sputtering target that prepared by the present embodiment is 99.8% of theoretical density.After testing, oxygen level is 495ppm.It can thus be appreciated that the density of tubulose molybdenum alloy sputtering target prepared by the present embodiment is high, product purity is high, and foreign matter content is low.
Embodiment 4
Composition graphs 1 and Fig. 2, the hot isostatic pressing preparation method of the present embodiment tubulose molybdenum alloy sputtering target comprises the following steps:
Step one, make hot isostatic pressing jacket according to the design requirements of tubulose molybdenum alloy sputtering target to be prepared; The external diameter of the hot isostatic pressing jacket made by the present embodiment is 290mm, internal diameter is 195mm, length is 3250mm, wall thickness is 4mm, opening for feed 3 is the circular hole of diameter 40mm, and mouth 4 of finding time is the circular hole of diameter 9mm, can weld an internal diameter 9mm in actual mechanical process at bleeding point 4 place, the titanium pipe of wall thickness 2.5mm, length 800mm is so that vacuum pumping;
Step 2, molybdenum alloy powder is loaded in hot isostatic pressing jacket by opening for feed 3 described in step one, sealing opening for feed 3 after jolt ramming on shaking platform; Described molybdenum alloy powder is preferably molybdenum niobium tantalum alloy powder, and wherein Mo is 80wt%, Nb be 10wt%, Ta is 10wt%; After jolt ramming, the relative density of molybdenum alloy powder is 54%;
Step 3, the bleeding point 4 of the hot isostatic pressing jacket that molybdenum alloy powder is housed in step 2 is connected vacuum pump, then put into retort furnace, be not more than 5 × 10 in vacuum tightness
-2pa, temperature is vacuum heat treatment 0.5h under the condition of 400 DEG C, carries out sealing after naturally cooling to bleeding point 4;
Step 4, the graphite core selecting diameter to be 204mm, core/sleeve is contained in the hot isostatic pressing jacket in step 3 after vacuum heat treatment, then hot isostatic pressing stove is put into, it is 1600 DEG C in temperature, pressure is hip moulding 2h under the condition of 150MPa, remove core after furnace cooling, from hot isostatic pressing jacket, take out moulding product, obtain tubulose molybdenum alloy sputtering target.
The internal diameter of tubulose molybdenum alloy sputtering target prepared by the present embodiment is 205mm, and wall thickness is 30mm, and length is 2400mm.After testing, the actual density of tubulose molybdenum alloy sputtering target that prepared by the present embodiment is 99.5% of theoretical density.After testing, oxygen level is 178ppm.It can thus be appreciated that the density of tubulose molybdenum alloy sputtering target prepared by the present embodiment is high, product purity is high, and foreign matter content is low.
Embodiment 5
Composition graphs 1 and Fig. 2, the hot isostatic pressing preparation method of the present embodiment tubulose molybdenum alloy sputtering target comprises the following steps:
Step one, make hot isostatic pressing jacket according to the design requirements of tubulose molybdenum alloy sputtering target to be prepared; The external diameter of the hot isostatic pressing jacket made by the present embodiment is 105mm, internal diameter is 35mm, length 1050mm, wall thickness is 1.5mm, opening for feed 3 is the circular hole of diameter 20mm, and mouth 4 of finding time is the circular hole of diameter 5mm, can weld an internal diameter 5mm in actual mechanical process at bleeding point 4 place, the titanium pipe of wall thickness 2mm, length 400mm is so that vacuum pumping;
Step 2, molybdenum alloy powder is loaded in hot isostatic pressing jacket by opening for feed 3 described in step one, sealing opening for feed 3 after jolt ramming on shaking platform; Described molybdenum alloy powder is preferably molybdenum-copper powder, and wherein Mo is 90wt%, Cu is 10wt%; After jolt ramming, the relative density of molybdenum alloy powder is 45.7%;
Step 3, the bleeding point 4 of the hot isostatic pressing jacket that molybdenum alloy powder is housed in step 2 is connected vacuum pump, then put into retort furnace, be not more than 5 × 10 in vacuum tightness
-2pa, temperature is vacuum heat treatment 4h under the condition of 150 DEG C, carries out sealing after naturally cooling to bleeding point 4;
Step 4, selection wall thickness are 10mm, the thick walled steel tube of external diameter 0.8mm less of the internal diameter of the first pipe fitting 1 is core, core/sleeve is contained in the hot isostatic pressing jacket in step 3 after vacuum heat treatment, then hot isostatic pressing stove is put into, be 800 DEG C in temperature, pressure is hip moulding 6h under the condition of 200MPa, removes core after furnace cooling, from hot isostatic pressing jacket, take out moulding product, obtain tubulose molybdenum alloy sputtering target.
The internal diameter of tubulose molybdenum alloy sputtering target prepared by the present embodiment is 40mm, and wall thickness is 20mm, and length is 900mm.After testing, the actual density of tubulose molybdenum alloy sputtering target that prepared by the present embodiment is 99.5% of theoretical density.After testing, oxygen level is 156ppm.It can thus be appreciated that the density of tubulose molybdenum alloy sputtering target prepared by the present embodiment is high, product purity is high, and foreign matter content is low.
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 (7)
1. a hot isostatic pressing preparation method for tubulose molybdenum alloy sputtering target, it is characterized in that, the method comprises the following steps:
Step one, require to make hot isostatic pressing jacket according to the shape and size of tubulose molybdenum alloy sputtering target to be prepared, described hot isostatic pressing jacket comprises the first pipe fitting (1) and is sleeved on the first pipe fitting (1) and second pipe fitting (2) coaxial with the first pipe fitting (1) outward, the lower end of described first pipe fitting (1) is connected by the first annular plate (5) with the lower end of the second pipe fitting (2), the upper end of described first pipe fitting (1) is connected by the second annular plate (6) with the upper end of the second pipe fitting (2), described second annular plate (6) offers opening for feed (3) and bleeding point (4),
Step 2, molybdenum alloy powder is loaded in hot isostatic pressing jacket by opening for feed described in step one (3), sealing opening for feed (3) after jolt ramming on shaking platform;
Step 3, will be equipped with in step 2 the hot isostatic pressing jacket of molybdenum alloy powder bleeding point (4) connect vacuum pump, be then placed in retort furnace, be not more than 5 × 10 in vacuum tightness
-2pa, temperature is vacuum heat treatment 0.5h ~ 4h under the condition of 150 DEG C ~ 400 DEG C, sealing bleeding point (4) after naturally cooling;
Step 4, be contained in core/sleeve in step 3 after vacuum heat treatment hot isostatic pressing jacket in, then the hot isostatic pressing jacket that core is housed is put into hot isostatic pressing stove, it is 800 DEG C ~ 1600 DEG C in temperature, pressure is hip moulding 2h ~ 6h under the condition of 150MPa ~ 200MPa, core is removed after furnace cooling, from hot isostatic pressing jacket, take out moulding product, obtain tubulose molybdenum alloy sputtering target.
2. the hot isostatic pressing preparation method of a kind of tubulose molybdenum alloy sputtering target according to claim 1, is characterized in that, the material of the first pipe fitting described in step one (1) and the second pipe fitting (2) is pure titanium or 20# steel.
3. the hot isostatic pressing preparation method of a kind of tubulose molybdenum alloy sputtering target according to claim 1, is characterized in that, the wall thickness of the first pipe fitting described in step one (1) and the second pipe fitting (2) is 1.5mm ~ 4mm.
4. the hot isostatic pressing preparation method of a kind of tubulose molybdenum alloy sputtering target according to claim 1, is characterized in that, the powder of molybdenum alloy described in step 2 is molybdenum niobium alloy powder, molybdenum niobium zirconium alloy powder, molybdenum niobium tantalum alloy powder or molybdenum-copper powder.
5. the hot isostatic pressing preparation method of a kind of tubulose molybdenum alloy sputtering target according to claim 1, it is characterized in that, the thick walled steel tube of to be wall thickness the be 10mm ~ 25mm of core described in step 4, the external diameter 0.5mm ~ 1mm less of the internal diameter of the first pipe fitting (1) of described core.
6. the hot isostatic pressing preparation method of a kind of tubulose molybdenum alloy sputtering target according to claim 1, it is characterized in that, core described in step 4 is cylindrical graphite bar, the diameter of section 0.5mm ~ 1mm less of the internal diameter of the first pipe fitting (1) of described core.
7. the hot isostatic pressing preparation method of a kind of tubulose molybdenum alloy sputtering target according to claim 1, it is characterized in that, the internal diameter of the molybdenum alloy sputtering target of tubulose described in step 4 is 40mm ~ 205mm, and the wall thickness of described tubulose molybdenum alloy sputtering target is 15mm ~ 30mm.
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| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
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| CN108866415B (en) * | 2018-06-11 | 2019-07-05 | 西安建筑科技大学 | A kind of high tough low-oxygen molybdenum alloy and preparation method |
| CN109048031A (en) * | 2018-08-21 | 2018-12-21 | 北京航空航天大学 | A kind of annular element hot isostatic pressing joint forming jacket |
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| CN110670032B (en) * | 2019-10-29 | 2021-10-01 | 金堆城钼业股份有限公司 | Molybdenum-nickel-copper multi-element alloy sputtering target material and preparation method thereof |
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