CN104148654A - Method for preparing target-level high-purity tantalum powder - Google Patents
Method for preparing target-level high-purity tantalum powder Download PDFInfo
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Abstract
The invention relates to a method for preparing target-level high-purity tantalum powder. According to the method for preparing the target-level high-purity tantalum powder, a block-shaped mixture of tantalum powder prepared through potassium fluotantalate sodium reduction and one or more of diluted slats including NaCl, KCl and KF is filtered and washed with pure water, when the conductivity of filtering and washing liquid is smaller than 5000 us/cm, the filtered and washed mixture is poured into a horizontal type ball mine for wet-type ball milling, the mixture is taken out, acid pickling, suction filtration and drying are conducted on the mixture, so that raw tantalum powder is obtained, thermal treatment, oxygen reduction, oxygen-reduction acid pickling, secondary drying and detection are conducted on the raw tantalum powder, and then the target-level high-purity tantalum powder is obtained. According to the method for preparing target-level high-purity tantalum powder, the technology is simple, the production cost is low, the tantalum powder prepared according to the method is large in apparent density, high in purity, low in oxygen content and capable of meeting the requirement of a target for the purity and the density of materials, and therefore tantalum target cost and tantalum alloy target cost are greatly reduced.
Description
Technical field
The present invention relates to nonferrous materials technical field, particularly relate to a kind of preparation method of target-grade High-purity Tantalum powder.
Background technology
In prior art, the preparation of tantalum target is to be mainly processed as master with tantalum ingot, and powder metallurgic method is with it easily obtains even aplitic texture, saves material, the advantage such as production efficiency height has become magnetic control spattering target another kind of main preparation methods and study hotspot.
The tantalum powder using as tantalum target must possess two important conditions: first purity is very high, generally more than 4N; Its two particle is preferably full particle, and apparent density is large, because cast aside the factor of texture, the density of tantalum target and the quality of tantalum target are closely bound up, and the quality of the higher tantalum target of density of tantalum target is better.
In view of These characteristics, except some are as the tantalum powder that adds element use, the best tantalum powder that powder metallurgic method is prepared tantalum target employing is electronics bombardment powder.But the production procedure of this tantalum powder raw material is long, cost of manufacture costliness, prepares further developing of tantalum target so limited powder metallurgy.
At present, also have some patented technologies that the acquisition pattern of tantalum powder is provided, lack but each tool is excellent:
Chinese patent CN102517460A provides a kind of method of purification and tantalum target of tantalum powder, and its technique comprises: low-purity tantalum powder is provided; Described low-purity tantalum powder is carried out to radio frequency heating purification.But the method has only realized the raising to tantalum powder purity.
Chinese patent CN102367568A provides a kind of manufacture craft of high-purity tantalum target, and tantalum powder is mixed; Pack mixed tantalum powder into mould; Cold moudling is vacuum heating-press sintering then.Here tantalum powder used is the porous tantalum powder of electronics bombardment powder or traditional three-dimensional UNICOM.Traditional tantalum powder preparation technique is not proposed to corrective measure targetedly.
Chinese patent CN102382993A provides a kind of preparation method of target-grade ultrahigh-purity metal, and the method has increased recrystallization technique in hydrometallurgy, effectively reduces the content of refractory metal impurity and radioactive element.The method is in the wet process of producing potassium floutaramite, to have found some new thinkings to improve the purity of tantalum powder.
Patent US6323055 has described a kind of method of preparing High-purity Tantalum, and High-purity Tantalum is produced and High-purity Tantalum sputtering target.The method comprises that purifying raw material refines High-purity Tantalum subsequently.The method is also the processing laying particular emphasis in the wet process of potassium floutaramite.
In prior art, also have in powder metallurgic method and prepare in tantalum target process and adopt electronics bombardment to prepare tantalum ingot, and then hydrogenation powder process.The method manufacturing cost is too high.
Summary of the invention
The object of the invention is to overcome the defect of above-mentioned prior art, a kind of tantalum powder internal voids that reduces is provided, effectively improve tantalum powder apparent density and purity, and technique is simple, the preparation method of the target-grade High-purity Tantalum powder that production cost is low.
For realizing the technical scheme that object of the present invention takes be:
A kind of preparation method of target-grade High-purity Tantalum powder, it is characterized in that its processing step is: the tantalum powder first sodium reduction potassium floutaramite being made and diluting salt mix lump material pure water diafiltration, in the time that the electrical conductivity of diafiltration liquid is less than 5000us/cm, pour the material after diafiltration into horizontal ball mill and carry out wet ball-milling, take out afterwards material and carry out pickling, suction filtration and oven dry and obtain the former powder of tantalum powder, then by former tantalum powder powder through Overheating Treatment, fall oxygen processing, fall oxygen pickling, again dry and detection obtains target-grade High-purity Tantalum powder;
One in NaCl, the KCl that above-mentioned diluting salt refers to and KF or several arbitrarily.
The described time with pure water diafiltration is 12～20 hours.
When described wet ball-milling, the weight ratio of material and ball is controlled at 1:2～5, and the solid-to-liquid ratio of material and pure water is controlled at 1:0.5～1.5, Ball-milling Time 4～8 hours.
The HNO that it is 5～15% that described pickling refers to by mass concentration
3, 1～5% H
2o
2with mix acid liquor pickling 2～4h of 0.2～2%HF, rear leaving standstill, then soak 1～3h.
Described oven dry refers under vacuum, 100～150 DEG C of conditions dries 10～15h.
First described heat treatment refer to processes 0.5～3h under 800～1000 DEG C of temperature conditions, is then slowly warming up to 1400～1550 DEG C and continues to process 0.5～3h, 10～20 DEG C/min of heating rate.
Described fall oxygen processing be adopt magnesium oxygen falls, in the tantalum powder after heat treatment, mix magnesium 0.5～3%, the argon filling of then finding time, is warming up to 8500～1000 DEG C (850), insulation reduce 1～3 hour, the row's of finding time magnesium 1～3 hour.
The described oxygen pickling HNO that refers to that to adopt mass concentration be 5～15% that falls
3carry out leaving standstill after pickling 2～4h with the mix acid liquor of 0.2～2%HF, and then soak 1～3h.
The present invention washes the rear ball mill of directly putting into by the block material water of mixing of tantalum powder that sodium reduction potassium floutaramite is made and diluting salt, add pure water to carry out wet ball-milling pulverizing simultaneously, original tantalum powder spongiform porous body can be destroyed like this, reduce porosity, the densification that it is become by loose structure; The impurity such as K, Na being simultaneously mingled with in porous body is also released, and removes by follow-up pickling process, has improved the purity of tantalum powder.Preparation method's technique of target-grade High-purity Tantalum powder of the present invention is simple, and production cost is low, and the tantalum powder apparent density of being prepared by the method is large, purity is high, oxygen content is low, has met the requirement of target to material purity and density, and then greatly reduces tantalum and tantalum alloy target cost.
Detailed description of the invention
Below in conjunction with example, the specific embodiment of the present invention is elaborated.It should be understood that example is for the present invention instead of limitation of the present invention are described.Scope of the present invention and core content are determined according to claims.
First tantalum powder sodium reduction potassium floutaramite being made relaxes block (dilution refers to one or more in NaCl, KCl and KF) with the lump material that mixes of dilution composition, first use pure water diafiltration 12～20 hours, in the time that the electrical conductivity of diafiltration liquid is less than 5000us/cm, pour the material after diafiltration into horizontal ball mill and carry out ball milling, the weight ratio of material and ball is controlled at 1:2～5, the solid-to-liquid ratio of material and pure water is controlled between 1:0.5～1.5, Ball-milling Time 4～8 hours.Then take out material and carry out pickling, the acid washing conditions is here to adopt the HNO that mass concentration is 5～15%
3, 1～5% H
2o
2carry out pickling 2～4h with the mix acid liquor of 0.2～2%HF, rear leaving standstill, then soak 1～3h, and then add pure water rinsing, suction filtration, under vacuum, dry (100～150 DEG C/10～15h) and get final product to obtain the former powder of tantalum powder.The former powder of this tantalum powder also will pass through (800～1000 DEG C/0.5～3h-1400～1550 DEG C/0.5～3h of normal subsequent heat treatment, 10～20 DEG C/min of heating rate), fall oxygen (adopt magnesium oxygen falls, in tantalum powder after heat treatment, mix magnesium 0.5～3%, then the argon filling of finding time, be warming up to 850～1000 DEG C, insulation is reduced 1～3 hour, the row's of finding time magnesium 1～3 hour), (the acid washing conditions is here to adopt the HNO that mass concentration is 5～15% to fall oxygen pickling, oven dry
3carry out leaving standstill after pickling 2～4h with the mix acid liquor of 0.2-2%HF, soak again 1-3h, then add pure water rinsing, suction filtration, under vacuum, dry (100～150 DEG C/10～15h)), the operation such as detection, the porosity that finally improved, improved apparent density and further carried highly purified fine and close High-purity Tantalum powder.
Embodiment 1:
Carry out the preparation of sodium reduction tantalum powder using NaCl as diluting salt, after finishing, reduction first the tantalum powder after sodium reduction is added to pure water diafiltration 10 hours with the lump material that mixes of diluting salt NaCl, in the time that the electrical conductivity of diafiltration liquid is 3000us/cm, show that the most salt in tantalum powder remove, then pour the material after diafiltration into horizontal ball mill and carry out ball milling, the weight ratio of material and ball is controlled at 1:2.5, and the solid-to-liquid ratio of material and pure water is controlled at 1:0.8, Ball-milling Time 5 hours.Then take out material and carry out pickling, acid solution consists of the HNO of mass concentration 10%
3, 2% H
2o
2, add 0.5%HF, after pickling 2h leave standstill, and then soak 1.5h, then add pure water rinsing, suction filtration suction filtration, under vacuum dry (120 DEG C/14h) get final product to obtain the former powder of tantalum powder.The former powder of this tantalum powder also will pass through (1000 DEG C/2h-1450 DEG C/1h of normal subsequent heat treatment, 10 DEG C/min of heating rate), falling oxygen (adopts magnesium to fall oxygen, in tantalum powder after heat treatment, mix magnesium 0.8%, then the argon filling of finding time, be warming up to 900 DEG C, insulation is reduced 3 hours, the row's of finding time magnesium 2 hours), oxygen pickling is fallen, (the acid washing conditions is here that mass concentration is 8% HNO3 in oven dry, after adding 0.3%HF pickling 2h, leave standstill, and then immersion 1h, then add pure water rinsing, suction filtration, under vacuum, dry (100 DEG C/15h), the operations such as detection, porosity has finally improved, improve apparent density and further carried highly purified fine and close High-purity Tantalum powder.
Embodiment 2:
Carry out the preparation of sodium reduction tantalum powder using KCl as diluting salt, after finishing, reduction first the tantalum powder after sodium reduction is added to pure water diafiltration 15 hours with the lump material that mixes of diluting salt KCl, in the time that the electrical conductivity of diafiltration liquid is 1500us/cm, show that the most salt in tantalum powder remove, then pour the material after diafiltration into horizontal ball mill and carry out ball milling, the weight ratio of material and ball is controlled at 1:4, and the solid-to-liquid ratio of material and pure water is controlled at 1:1, Ball-milling Time 8 hours.Then take out material and carry out pickling, acid solution consists of the HNO of mass concentration 8%
3, 3% H
2o
2, add after 0.7%HF pickling 2.5h and leave standstill, and then soak 1h, then add pure water rinsing, suction filtration suction filtration, under vacuum, dry (150 DEG C/12h) and get final product to obtain the former powder of tantalum powder.The former powder of this tantalum powder also will pass through (1000 DEG C/2h-1480 DEG C/1.5h of normal subsequent heat treatment, 15 DEG C/min of heating rate), falling oxygen (adopts magnesium to fall oxygen, in tantalum powder after heat treatment, mix magnesium 1.2%, then the argon filling of finding time, be warming up to 920 DEG C, reductase 12 .5 hour is carried out in insulation, the row's of finding time magnesium 1.5 hours), oxygen pickling is fallen, (the acid washing conditions is here that mass concentration is 10% HNO3 in oven dry, after adding 0.5%HF pickling 1.5h, leave standstill, and then immersion 1h, then add pure water rinsing, suction filtration, under vacuum, dry (100 DEG C/15h), the operations such as detection, porosity has finally improved, improve apparent density and further carried highly purified fine and close High-purity Tantalum powder.
Embodiment 3:
Carry out the preparation of sodium reduction tantalum powder as diluting salt using the salt-mixture of KCl and NaCl, after finishing, reduction first the tantalum powder after sodium reduction is added to pure water diafiltration 20 hours with the lump material that mixes of diluting salt KCl and NaCl, in the time that the electrical conductivity of diafiltration liquid is 1000us/cm, show that the most salt in tantalum powder remove, then pour the material after diafiltration into horizontal ball mill and carry out ball milling, the weight ratio of material and ball is controlled at 1:5, the solid-to-liquid ratio of material and pure water is controlled at 1:1.5, Ball-milling Time 9 hours.Then take out material and carry out pickling, acid solution consists of the HNO of mass concentration 10%
3, 2% H
2o
2, add after 0.5%HF pickling 2h and leave standstill, and then soak 1.5h, then add pure water rinsing, suction filtration suction filtration, under vacuum, dry (120 DEG C/14h) and get final product to obtain the former powder of tantalum powder.The former powder of this tantalum powder also will pass through (1000 DEG C/2h-1450 DEG C/1h of normal subsequent heat treatment, 10 DEG C/min of heating rate), falling oxygen (adopts magnesium to fall oxygen, in tantalum powder after heat treatment, mix magnesium 0.8%, then the argon filling of finding time, be warming up to 900 DEG C, insulation is reduced 3 hours, the row's of finding time magnesium 2 hours), oxygen pickling is fallen, (the acid washing conditions is here that mass concentration is 8% HNO3 in oven dry, after adding 0.3%HF pickling 2h, leave standstill, and then immersion 1h, then add pure water rinsing, suction filtration, under vacuum, dry (100 DEG C/15h), the operations such as detection, porosity has finally improved, improve apparent density and further carried highly purified fine and close High-purity Tantalum powder.
Comparative example 4:
Carry out the preparation of sodium reduction tantalum powder using the salt-mixture of KCl and NaCl as diluting salt, after reduction finishes, the tantalum powder after sodium reduction is added to pure water diafiltration 20 hours with the lump material that mixes of diluting salt KCl and NaCl, in the time that the electrical conductivity of diafiltration liquid is 1000us/cm.Then take out material and carry out pickling, acid solution consists of the HNO of mass concentration 10%
3, 2% H
2o
2, add after 0.5%HF pickling 2h and leave standstill, and then soak 1.5h, then add pure water rinsing, suction filtration suction filtration, under vacuum, dry (120 DEG C/14h) and get final product to obtain the former powder of tantalum powder.The former powder of this tantalum powder also will pass through (1000 DEG C/2h-1450 DEG C/1h of normal subsequent heat treatment, 10 DEG C/min of heating rate), falling oxygen (adopts magnesium to fall oxygen, in tantalum powder after heat treatment, mix magnesium 0.8%, then the argon filling of finding time, be warming up to 900 DEG C, insulation is reduced 3 hours, the row's of finding time magnesium 2 hours), oxygen pickling is fallen, (the acid washing conditions is here that mass concentration is 8% HNO3 in oven dry, after adding 0.3%HF pickling 2h, leave standstill, and then immersion 1h, then add pure water rinsing, suction filtration, under vacuum, dry (100 DEG C/15h), the operations such as detection, finally obtain the tantalum powder of normal process.
Example 1, example 2, example 3, comparative example 4 are analyzed, and result is as follows:
Table 1: the physical properties of tantalum powder
| Sample | Porosity (%) | Fsss(μm) | SBD(g/cc) | +80(％) | -400(％) |
| Example 1 | 38 | 6.54 | 3.12 | 0.00 | 85.86 |
| Example 2 | 36 | 6.68 | 3.08 | 0.00 | 83.12 |
| Example 3 | 35 | 6.36 | 3.28 | 0.00 | 88.16 |
| Comparative example 4 | 56 | 5.58 | 2.42 | 0.20 | 41.30. |
In this table, (μ m) represents Fei Shi particle diameter to Fsss, SBD (g/cc) represents apparent density, and+80 (%) represents to be greater than the shared ratio of 80 object tantalum powder, and-400 (%) represents to be less than the shared ratio of 400 object tantalum powder.
Example 1, example 2, example 3 porosity compared with comparative example 4 reduces as can be seen from Table 1, and apparent density has had increase, and fine powder ratio (400 order) significantly increases, and original loose structure is broken, and it is finer and close that powder becomes.Meet the feature that target tantalum powder porosity is low, density is higher.
Table 2: major impurity content in tantalum powder (unit: ppm)
In upper table, in tantalum powder, the detection method of element all derives from the national standards such as GB/T15076.8-2008, GB/T15076.9-2008, GB/T15076.12-2008, GB/T15076.14-2008, GB/T15076.15-2008, GB/T15076.16-2008, " tantalum niobium chemical analysis method ".
Example 1, example 2, example 3 oxygen, carbon, iron equal size compared with comparative example 4 has reduction in various degree as can be seen from Table 2, met the high-purity feature of target tantalum powder.
Claims (8)
1. the preparation method of a target-grade High-purity Tantalum powder, it is characterized in that its processing step is: the tantalum powder first sodium reduction potassium floutaramite being made and diluting salt mix lump material pure water diafiltration, in the time that the electrical conductivity of diafiltration liquid is less than 5000us/cm, pour the material after diafiltration into horizontal ball mill and carry out wet ball-milling, take out afterwards material and carry out pickling, suction filtration and oven dry and obtain the former powder of tantalum powder, then by former tantalum powder powder through Overheating Treatment, fall oxygen processing, fall oxygen pickling, again dry and detection obtains target-grade High-purity Tantalum powder;
One in NaCl, the KCl that above-mentioned diluting salt refers to and KF or several arbitrarily.
2. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, it is characterized in that the described time with pure water diafiltration is 12～20 hours.
3. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, while it is characterized in that described wet ball-milling, the weight ratio of material and ball is controlled at 1:2～5, and the solid-to-liquid ratio of material and pure water is controlled at 1:0.5～1.5, Ball-milling Time 4～8 hours.
4. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, it is characterized in that the described pickling HNO that to refer to by mass concentration be 5～15%
3, 1～5% H
2o
2with mix acid liquor pickling 2～4h of 0.2～2%HF, rear leaving standstill, then soak 1～3h.
5. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, it is characterized in that described oven dry refers under vacuum, 100～150 DEG C of conditions to dry 10～15h.
6. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, it is characterized in that first described heat treatment refer to processes 0.5～3h under 800～1000 DEG C of temperature conditions, then be slowly warming up to 1400～1550 DEG C and continue to process 0.5～3h, 10～20 DEG C/min of heating rate.
7. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, described in it is characterized in that, falling oxygen processing is to adopt magnesium to fall oxygen, in tantalum powder after heat treatment, mix magnesium 0.5～3%, then the argon filling of finding time, be warming up to 850 DEG C～1000 DEG C, insulation is reduced 1～3 hour, the row's of finding time magnesium 1～3 hour.
8. according to the preparation method of target-grade High-purity Tantalum powder claimed in claim 1, the HNO that oxygen pickling refers to that employing mass concentration is 5～15% falls described in it is characterized in that
3carry out leaving standstill after pickling 2～4h with the mix acid liquor of 0.2～2%HF, and then soak 1-3h.
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| CN105458278A (en) * | 2015-12-08 | 2016-04-06 | 贵研铂业股份有限公司 | Preparation method of high-purity spherical ruthenium powder |
| CN112317754A (en) * | 2020-11-18 | 2021-02-05 | 贵州振华电子信息产业技术研究有限公司 | Sheet ball-milling tantalum powder and preparation method and application thereof |
| 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 |
| CN114749655A (en) * | 2022-04-29 | 2022-07-15 | 宁夏东方钽业股份有限公司 | High-purity tantalum powder and preparation method thereof |
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| CN103894601A (en) * | 2014-04-23 | 2014-07-02 | 宁夏东方钽业股份有限公司 | Preparation method of high-pressure tantalum powder with improved voltage resistance performance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| CN114749655B (en) * | 2022-04-29 | 2023-10-24 | 宁夏东方钽业股份有限公司 | High-purity tantalum powder and preparation method thereof |
| WO2023206905A1 (en) * | 2022-04-29 | 2023-11-02 | 宁夏东方钽业股份有限公司 | High-purity tantalum powder and preparation method therefor |
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