CN102658346A - Forging method of large tantalum targets - Google Patents
Forging method of large tantalum targets Download PDFInfo
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- CN102658346A CN102658346A CN2012100989359A CN201210098935A CN102658346A CN 102658346 A CN102658346 A CN 102658346A CN 2012100989359 A CN2012100989359 A CN 2012100989359A CN 201210098935 A CN201210098935 A CN 201210098935A CN 102658346 A CN102658346 A CN 102658346A
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Abstract
A forging method of large tantalum targets is used to homogenize the large tantalum targets by forging means of squaring, drawing, rounding and upsetting and intermediate thermal treatment, and includes the steps of firstly, squaring and drawing; secondly, sawing material at fixed length according to 2-2.5 times of a finished product in weight; thirdly, acid washing; fourthly, thermally treating at the temperature 25%-50% of that of melting point of tantalum, and holding the temperature for 60-150 minutes; fifthly, secondary forging, namely upsetting, and coating upper plane and lower plane with lubricant during upsetting; sixthly, acid washing the same as that in step 3; seventhly, thermal treatment the same as that in the step 4; and eighthly, tertiary forging, namely using a precision forging machine to round a blank.
Description
Technical field
The present invention relates to the magnetic control spattering target technology, particularly a kind of forging method of big specification tantalum target.
Background technology
Physical vapor deposition (PVD) is one of technology of most critical in the semiconductor chip production process; Its objective is and deposit to the form of the compound of metal or metal on silicon chip or other the substrate with film; And, finally form distribution structure complicated in the semiconductor chip subsequently through the cooperating of technologies such as photoetching and corrosion.Physical vapour deposition (PVD) is accomplished through the sputter board, and sputtering target material is exactly a very important crucial consumptive material that is used for above-mentioned technology.Common sputtering target material has high-purity Ta, also has non-ferrous metals such as Ti, Al, Co and Cu.The production of sputtering target material is developed evolution simultaneously with production process of semiconductor, so the information of aspects such as its production technology and application is very rare.And because the high investment of semiconductor technology, excessive risk and high competition property cause with information such as the technology of the closely bound up target of its competitiveness (being determined by cost and technology), markets very secret.The whole world has only Japan, two countries of the U.S. to possess the production capacity of production semiconductor with advanced sputtering target material at present, and in Taiwan, although Korea S's semiconductor production is very capable, target still relies on the import by the U.S. and Japan.
Fast development along with semiconductor technology; Integrated degree is increasingly high, and unit are monocrystalline silicon piece integrator number of packages is exponential increase, and die size is also increasing; Wiring width is more and more thinner; Thereby also increasing to the dimensional requirement of sputtering target material, heterogeneous microstructure also requires more and more meticulousr, the forward position of semiconductor technology is exactly 12 at present " wafer super large-scale integration manufacturing technology.
The wafer target with the need of 8 " target is exactly corresponding production 8 "." wafer 90nm technology; what researching and developing is 65nm, 45nm, 32nm technology, China's large-scale production at present are to be " wafer 0.13-0.18um (130-180nm) technology that is 8 of representative with the SMIC though at present the forward position of world semiconductor integrated circuit is 12.
Along with wafer size increases to 300mm (12 inches) from 200mm (8 inches); Corresponding sputtering target material size must increase the basic demand that could satisfy the PVD plated film thereupon, and simultaneously, live width is reduced to 90-45nm from (130-180nm); Based on the electric conductivity of conductor and the matching performance of barrier layer; Then sputtering target material will be to be converted into ultra-pure Cu/Ta to be from ultra-pure Al/Ti also, and the Ta target is increasing in the importance of semiconductor sputter industry, and demand is also increasing simultaneously.
The uniformity of silicon chip upper film thickness after the sputter; Be very important concerning final products; This depends on interior tissue and the texture orientation of tantalum target, uniform crystal particles refinement, the target that crystal grain crystalline orientation convergence is identical, in sputter, can make identical by the crystal grain sputter rate convergence of sputter, sputtered atom angle distribution track convergence is identical; Will obtain the coating of film thickness uniformity like this, the material utilization rate of tantalum target also is largely increased simultaneously.
China still is in the immature stage in the technology of producing big specification (8 inches or 12 inches) tantalum target at present.The major defect of prior art is: for large scale (diameter is greater than 200mm) ingot, can not be effectively after the forging even broken former crystal grain, produce defectives such as crystal zone and crystal grain is inhomogeneous.
Summary of the invention
The objective of the invention is to overcome the prior art defective, a kind of forging method of big specification tantalum target is provided.
The object of the invention is realized according to following proposal:
A kind of forging method of big specification tantalum target is characterized in that it being to adopt the side of beating to pull out, beat circle, jumping-up forging means, the middle heat-treating methods that cooperates, and realizes homogenizing of big specification tantalum target;
One of concrete steps are: the first step, the side's of beating pulling; In second step, scale saw material calculates according to 2～2.5 times of weight of final finished, the saw material; The 3rd step, pickling; The 4th step, heat treatment, heat treatment temperature is 25%～50% of a tantalum material fusing point, temperature retention time is 60～150min; In the 5th step, secondary forges, jumping-up, and when jumping-up, last lower plane is coated with lubricating oil; In the 6th step, pickling is with the 3rd step; The 7th step, heat treatment, with the 4th step, in the 8th step, circle is beaten in three forgings, with precise forging machine blank is looked for circle;
Two of concrete steps are: the first step: scale saw material, calculate the saw material by 2～2.5 times of weight of final finished; In second step, once forge jumping-up, H/D=1.0～1.5; The 3rd step: pickling; The 4th step, heat treatment, heat treatment temperature is 35%～50% of a tantalum material fusing point, temperature retention time is 60～120min; In the 5th step, secondary forges, the side's of beating pulling; The 6th step, pickling; In the 7th step, heat treatment is with the 4th step; The 8th step, three forgings, jumping-up is beaten circle before the jumping-up; The 9th step, pickling; The tenth step: heat treatment, with the 4th step;
Hydrochloric acid, hydrofluoric acid are adopted in above-mentioned pickling, and its volume ratio is: HCl: HF: H
2O=5: 2: 3 removes surface impurity, and the visible tantalum metallic luster of perusal does not have assorted spot and gets final product.
Because China's economic has experienced the high speed development in more than 20 year; Not only attract foreign vendor with low production cost; Attracted simultaneously the sight of global semiconductor industry again with great demand, China is semiconductor industry country with the fastest developing speed in the world, world semiconductor industry forward China migration at present; From Intel to IBM,, all found the factory to China one after another to the foundry giant in Taiwan.China is just rising and is taking turns the peak that semiconductor is founded the factory.According to estimates, to China, set up 4 from the fund input that at present hundred million dollars of hundreds ofs will be arranged to a few years from now on ", 5 ", 6 ", 8 " and 12 " production line.Will form huge production capacity when the time comes.Thereby China and Asia semiconductor chip manufacture will be very huge to the demand of sputtering target material.
The present invention adopts new Forging Technology; Be equipped with proper heat treatment technology, near the fine grained region the columnar zone in the ingot casting, center equiax crystal district and the tantalum ingot edge is implemented effectively fragmentation, the metal flow of blank core increases; The degree of irregularity of central tissue significantly improves; Under multi-direction stressed situation, make its original as cast condition open grain structure obtain multi-faceted abundant fragmentation, like this; Impel the forging and pressing slab to obtain the relative uniform tissue of crystal grain, avoided central part not to be implemented into effective fragmentation and the existence of harmful tissues such as follow-up leaving over down " crystal zone " tissue and open grain structure.
The specific embodiment
Embodiment 1
8 " the forging step of tantalum target
First step: once forge the side's of beating pulling, Φ 150mm * L → 100mm * 100mm * L ˊ; Forge feed L=0.8h, (h is the height of blank before forging), drafts Δ h=0.15h; For obtaining distortion comparatively uniformly, when the pulling operation, interlaced the opening of feed entrance point in the time of should making front and back each time compression; Controlled in order to guarantee to depress unanimity at every turn, adopt standard gauge block as cushion block.
Second step: scale saw material, calculate the saw material according to 2～2.5 times of weight of final finished;
Third step: pickling, HCl: HF: H
2O=5: 2: 3 (volume ratio) removes surface impurity, and the visible tantalum metallic luster of perusal does not have assorted spot and gets final product;
The 4th step: heat treatment, heat treatment temperature are 25%～50% of tantalum material fusing point, and temperature retention time is 60～150min;
The 5th step: secondary forges, jumping-up, and 100mm * 100mm → 210mm * 210mm, when jumping-up, last lower plane is coated with lubricating oil.
The 6th step: pickling, same step 3;
The 7th step: heat treatment, same step 4.
The 8th step: three forgings, look for circle, with precise forging machine blank is looked for round Φ 240mm.
Embodiment 2
12 " the forging step of tantalum target
First step: scale saw material,, calculate the saw material according to different user demands by 2～2.5 times of weight of final finished;
Second step: once forge, jumping-up, H/D=1.0～1.5, during jumping-up, upper and lower surfaces is coated with lubriation material;
Third step: pickling, HCl: HF: H
2O=5: 2: 3 (volume ratio) removes surface impurity, and the visible tantalum metallic luster of perusal does not have assorted spot and gets final product;
The 4th step: heat treatment, heat treatment temperature are 35% ~ 50% of tantalum material fusing point, and temperature retention time is 60～120min;
The 5th step: secondary forges, the side's of beating pulling, 150mm * 150mm * L; Forge feed L=0.6～0.8h, (h is the height of blank before forging), drafts Δ h=0.12～0.15h; For obtaining distortion comparatively uniformly, when the pulling operation, interlaced the opening of feed entrance point in the time of should making front and back each time compression; Controlled in order to guarantee to depress unanimity at every turn, adopt standard gauge block as cushion block.
The 6th step: pickling, same step 3;
The 7th step: heat treatment, same step 4;
The 8th step: three forgings, jumping-up is beaten circle before the jumping-up.Φ 120mm → Φ 280mm, when jumping-up, last lower plane is coated with lubriation material;
The 9th step: pickling, same step 3;
The tenth step: heat treatment, same step 4.
Claims (4)
1. the forging method of a big specification tantalum target is characterized in that it being to adopt the side of beating to pull out, beat circle, jumping-up forging means, and the middle heat-treating methods that cooperates is realized homogenizing of big specification tantalum target.
2. the forging method of big specification tantalum target as claimed in claim 1 is characterized in that concrete steps are: the first step, the side's of beating pulling; In second step, scale saw material calculates according to 2～2.5 times of weight of final finished, the saw material; The 3rd step, pickling; The 4th step, heat treatment, heat treatment temperature is the 25%-50% of tantalum material fusing point, temperature retention time is 60～150min; In the 5th step, secondary forges, jumping-up, and when jumping-up, last lower plane is coated with lubricating oil; In the 6th step, pickling is with the 3rd step; The 7th step, heat treatment, with the 4th step, in the 8th step, circle is beaten in three forgings, with precise forging machine blank is looked for circle.
3. the forging method of big specification tantalum target as claimed in claim 1 is characterized in that concrete steps are: the first step: scale saw material, calculate the saw material by 2～2.5 times of weight of final finished; In second step, once forge jumping-up, H/D=1.0～1.5; The 3rd step: pickling; The 4th step, heat treatment, heat treatment temperature is 35%～50% of a tantalum material fusing point, temperature retention time is 60～120min; In the 5th step, secondary forges, the side's of beating pulling; The 6th step, pickling; In the 7th step, heat treatment is with the 4th step; The 8th step, three forgings, jumping-up is beaten circle before the jumping-up; The 9th step, pickling; The tenth step: heat treatment, with the 4th step.
4. like the forging method of claim 2 or 3 described big specification tantalum targets, it is characterized in that above-mentioned pickling employing hydrochloric acid, hydrofluoric acid, its volume ratio is: HCl: HF: H
2O=5: 2: 3 removes surface impurity, and the visible tantalum metallic luster of perusal does not have assorted spot and gets final product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102921850A (en) * | 2012-10-31 | 2013-02-13 | 宁夏东方钽业股份有限公司 | Tantalum decatungstate bar and production method for same |
| CN104451567A (en) * | 2014-12-29 | 2015-03-25 | 宁夏东方钽业股份有限公司 | Tantalum target and manufacturing method thereof |
| CN104532196A (en) * | 2014-12-10 | 2015-04-22 | 宁夏东方钽业股份有限公司 | Method for forging tantalum target |
| CN113025972A (en) * | 2021-03-01 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Manufacturing method of aluminum target material |
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| CN113025972A (en) * | 2021-03-01 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Manufacturing method of aluminum target material |
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Application publication date: 20120912 |