CN103447544B - Size distribution concentrates controlled High-purity Tantalum powder, preparation method thereof - Google Patents
Size distribution concentrates controlled High-purity Tantalum powder, preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of size distribution and concentrate controlled High-purity Tantalum powder, preparation method thereof, comprise: High-purity Tantalum ingot is hydrogenated to tantalum chip, put into pulverizer and beat pulverizing in unlimited mode, then sieve, tantalum powder under sieve carries out higher-order of oscillation classification, again low-temperature vacuum drying is carried out to the tantalum powder after classification, finally dehydrogenation is carried out to tantalum powder; Wherein, at least in pulverizing, classification process, the utensil contacted with tantalum powder all adopts the tantalum of purity more than 99.99% to make.Preferably, in classification process, adopt selected liquid as medium.By technique of the present invention, tantalum powder in process of production, because all adopting high prefect dielectric, seldom brings new impurity into, do not need follow-up pickling or other purifying techniques, shorten technological process, economy is environmental protection again, and tantalum powder low-carbon (LC), hypoxemia, low impurity, during classification, liquid medium directly contacts with tantalum powder, prevent the surface adhesion of thickness tantalum powder, the tantalum powder particles after classification is clean, and centralized particle diameter is controlled.
Description
Technical field
The present invention relates to a kind of preparation method of tantalum powder, be specifically related to the broken classification of a kind of High-purity Tantalum ingot hydrogenation and produce the method that size distribution concentrates controlled High-purity Tantalum powder.
Background technology
Industrial technical field, along with the development of semiconductor technology, computer chip integration degree is more and more higher, after chip live width enters 90 ~ 45nm field, Cu in Cu plated film can carry out atoms permeating to Si sheet, for a change this phenomenon, and chip coating process adopts Ta to be used as the barrier material preventing Cu from spreading to Si, be developed to Cu/Ta system by Al/Ti system with sputtering target material, the demand of tantalum spattering target also rolls up.Tantalum spattering target can be machined into by High-purity Tantalum ingot, also can be prepared by hot pressed sintering with tantalum powder.Sputtering target is produced in the hot pressing of tantalum powder not only can reduce mechanical processing difficulty, can also eliminate the intrinsic texture band of tantalum, produce the film that the uniformity is higher in sputtering.Tantalum powder for tantalum spattering target is generally pulverized with the hydrogenation of high-purity tantalum ingot and obtains.Tantalum ingot hydrogenation powder also occupies a tiny space in producing at another important applied field-tantalum electric capacity of tantalum, is particularly widely used in middle high-pressure tantalum electric capacity is produced.
In high-purity tantalum ingot hydrogenation pulverizing process, ball mill grinding be carried out, C, O and other metal impurities in this process, can be brought into, follow-up acid need be carried out and invade and magnesium-reduced process, to reduce C, O and the metal impurities brought into are produced in removal.The tantalum powder produced also needs to carry out classification process, and the general multi-scale analysis that adopts sieves technology or cyclone classified technology.These two kinds of classification techniques all have its limitation, and classification is not thorough, and the tantalum powder domain size distribution of acquisition is concentrated not.
Summary of the invention
A kind of size distribution is the object of the present invention is to provide to concentrate controlled High-purity Tantalum powder, preparation method thereof, it does not increase C and other impurity contents producing in tantalum powder process, oxygen content reduces, and the tantalum powder particles produced is clean, centralized particle diameter is controlled, thus overcomes deficiency of the prior art.
For achieving the above object, present invention employs following technical scheme:
Size distribution concentrates a controlled High-purity Tantalum powder, preparation method thereof, comprising: after High-purity Tantalum ingot is hydrogenated to tantalum chip, carries out successively pulverizing, classification, then the tantalum powder after classification is carried out low-temperature vacuum drying and Dehydroepiandrosterone derivative successively;
Wherein, at least in pulverizing, classification process, the utensil contacted with tantalum powder all adopts the tantalum of purity more than 99.99% to make.
As one of comparatively preferred embodiment, in crushing process, adopt the grinding mode of open type.
As one of comparatively preferred embodiment, in classification process, adopt selected liquid as medium.
Further, described selected liquid comprises ethanol, and is not limited thereto.
As one of comparatively preferred embodiment, in classification process, use higher-order of oscillation grading technology.
As one of comparatively preferred embodiment, this preparation method can comprise: High-purity Tantalum ingot is heated to more than 700 DEG C in hydrogenation furnace, with purity 99.999% hydrogen be hydrogenated to tantalum chip.
A kind of size distribution concentrates controlled High-purity Tantalum powder, preparation method thereof, comprise: High-purity Tantalum ingot is hydrogenated to tantalum chip, put into pulverizer and beat pulverizing in unlimited mode, then sieve, tantalum powder under sieve carries out higher-order of oscillation classification, again low-temperature vacuum drying is carried out to the tantalum powder after classification, finally dehydrogenation is carried out to tantalum powder;
Wherein, at least in pulverizing, classification process, the utensil contacted with tantalum powder all adopts the tantalum of purity more than 99.99% to make.
As one of comparatively preferred embodiment, in classification process, adopt selected liquid as medium, described selected liquid comprises ethanol.
As one of comparatively preferred embodiment, in the process of sieving, the analysis sieve net lattice of employing are 200-2000 order.
As one of comparatively preferred embodiment, the temperature of low-temperature vacuum drying is below 150 DEG C.
As one of comparatively preferred embodiment, the process conditions of dehydrogenation comprise: tantalum powder is heated to more than 800 DEG C in hydrogenation furnace and carries out dehydrogenation.
Compared with prior art, the present invention at least has following beneficial effect:
1, tantalum powder beat pulverizing and classification process in all adopt the tantalum of purity more than 99.99% to make with the utensil of powder contact, can reduce as far as possible or avoid to bring new impurity into, do not need follow-up pickling or other purifying techniques, shorten technological process, economy is environmental protection again, and tantalum powder low-carbon (LC), hypoxemia, low impurity;
2, be different from traditional ball mill grinding, adopt the grinding mode of open type, avoid hydrogen on the impact of tantalum medium;
3, classification process adopts higher-order of oscillation technology, and using liquid as medium, medium directly contacts with tantalum powder, prevents the surface adhesion of thickness tantalum powder, and the tantalum powder particles after classification is clean, and centralized particle diameter is controlled.
Accompanying drawing explanation
Fig. 1 be a preferred embodiment of the present invention obtain the grain size distribution of the controlled High-purity Tantalum powder of granularity;
Fig. 2 be a preferred embodiment of the present invention obtain the stereoscan photograph of the controlled High-purity Tantalum powder of granularity.
Detailed description of the invention
Below in conjunction with accompanying drawing and a preferred embodiment, technical scheme of the present invention is further described.
embodiment 1high-purity Tantalum ingot is heated to 700 DEG C in hydrogenation furnace, with purity 99.999% hydrogen be hydrogenated to tantalum chip.Again the tantalum chip of 1.6 kilograms is loaded in pulverizer tantalum crucible and carry out beaing pulverizing, grinding time 2 minutes.The tantalum powder vibration screening pulverized, analysis sieve net lattice are 325 orders, load in tantalum cup, inject 600ml absolute alcohol by lower for 0.8 kilogram of sieve tantalum powder, carry out higher-order of oscillation classification, repeatedly, after classification, tantalum powder carries out low-temperature vacuum drying in classification, baking temperature 150 DEG C, last tantalum powder is heated to 800 DEG C and carries out dehydrogenation in hydrogenation furnace, after dehydrogenation, the chemical constituent analysis of tantalum powder is as table 1, and domain size distribution is as Fig. 1, and ESEM is as Fig. 2.
By technique of the present invention, tantalum powder in process of production, adopts high prefect dielectric because of whole, seldom bring new impurity into, do not need follow-up pickling or other purifying techniques, shorten technological process, economy is environmental protection again, and tantalum powder low-carbon (LC), hypoxemia, low impurity, during classification, liquid medium directly contacts with tantalum powder, prevents the surface adhesion of thickness tantalum powder, tantalum powder particles after classification is clean, and centralized particle diameter is controlled.
It should be noted that; as described above is only the preferred embodiment explaining the present invention; not attempt does any restriction in form to the present invention according to this; be with; all any modification or changes having the relevant the present invention that does under identical invention spirit, all must be included in the category that the invention is intended to protection.
table 1 embodiment 1 obtain the chemical constituent analysis of tantalum powder after dehydrogenation
| Project | Result (μ g/g) | Project | Result (μ g/g) |
| C | 26 | Mo | 0.8 |
| O | 620 | Mn | 0.4 |
| N | 20 | Nb | 1.6 |
| H | 10 | Co | 0.1 |
| Li | <0.008 | Ti | 0.6 |
| Pb | <0.03 | Ni | 0.8 |
| Na | 0.7 | Zr | 0.6 |
| Cu | 0.1 | Fe | 1.6 |
| K | <0.3 | Hf | 0.02 |
| Zn | 0.3 | Cr | 0.8 |
| Mg | 0.1 | V | <0.009 |
| Cd | <0.03 | Si | 2.0 |
| Ca | <0.1 | Sn | <0.05 |
| W | 1.6 | U | <0.005 |
| Al | 0.3 | Th | <0.005 |
Claims (2)
1. a size distribution concentrates controlled High-purity Tantalum powder, preparation method thereof, it is characterized in that, comprise: High-purity Tantalum ingot is heated to more than 700 DEG C in hydrogenation furnace, with purity 99.999% hydrogen be hydrogenated to tantalum chip, put into pulverizer and beat pulverizing in unlimited mode, then sieve, in the process of sieving, the analysis sieve net lattice adopted are 200-2000 order, tantalum powder under sieve carries out higher-order of oscillation classification, adopt selected liquid as medium, then low-temperature vacuum drying is carried out to the tantalum powder after classification, finally dehydrogenation is carried out to tantalum powder;
Wherein, at least in pulverizing, classification process, the utensil contacted with tantalum powder all adopts the tantalum of purity more than 99.99% to make;
The temperature of low-temperature vacuum drying is below 150 DEG C, and the process conditions of dehydrogenation comprise: tantalum powder is heated to more than 800 DEG C in hydrogenation furnace and carries out dehydrogenation.
2. size distribution according to claim 1 concentrates controlled High-purity Tantalum powder, preparation method thereof, it is characterized in that, described selected liquid comprises ethanol.
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| EP3112059B1 (en) * | 2014-02-27 | 2020-01-15 | Ningxia Orient Tantalum Industry Co., Ltd. | Preparation of high-purity tantalum powder |
| CN106735254B (en) * | 2016-12-28 | 2019-08-16 | 宁夏东方钽业股份有限公司 | A kind of metal powder and its preparation method and application |
| CN108788129B (en) * | 2018-06-29 | 2021-07-06 | 宁夏东方钽业股份有限公司 | Refractory metal powder, preparation method thereof and metal product |
| CN113981390A (en) * | 2021-10-29 | 2022-01-28 | 宁波江丰半导体科技有限公司 | Preparation method of high-purity low-oxygen tantalum target material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035852A (en) * | 1988-03-18 | 1989-09-27 | 中南工业大学 | Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction |
| CN102909365A (en) * | 2012-11-20 | 2013-02-06 | 重庆润泽医药有限公司 | Medical tantalum powder and preparation method thereof |
| CN103084196A (en) * | 2012-12-31 | 2013-05-08 | 北京科技大学 | Preparation method and application of tantalum-based hierarchical structure hollow nanometer photocatalytic material |
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| JP2006278031A (en) * | 2005-03-28 | 2006-10-12 | Mitsubishi Chemicals Corp | Manufacturing method of cathode material for lithium secondary battery and cathode material for lithium secondary battery as well as cathode for lithium secondary battery and lithium secondary battery using the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035852A (en) * | 1988-03-18 | 1989-09-27 | 中南工业大学 | Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction |
| CN102909365A (en) * | 2012-11-20 | 2013-02-06 | 重庆润泽医药有限公司 | Medical tantalum powder and preparation method thereof |
| CN103084196A (en) * | 2012-12-31 | 2013-05-08 | 北京科技大学 | Preparation method and application of tantalum-based hierarchical structure hollow nanometer photocatalytic material |
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