CN104148654B - A kind of preparation method of the high-purity tantalum powder of target-grade - Google Patents
A kind of preparation method of the high-purity tantalum powder of target-grade Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of the high-purity tantalum powder of target-grade, the technique uses the mixing block material pure water diafiltration by one of tantalum powder and NaCl, KCl and KF made from sodium reduction potassium floutaramite or any several diluting salts, when the conductivity of diafiltration liquid is less than 5000us/cm, material after diafiltration is poured into horizontal ball mill and carries out wet ball-milling, take out that material carries out pickling, suction filtration and drying obtain tantalum powder original powder later, then by tantalum powder original powder through Overheating Treatment, the processing of drop oxygen, drop oxygen pickling, drying and detection obtain the high-purity tantalum powder of target-grade again.Present invention process is simple, and production cost is low, and the tantalum powder apparent density prepared by this method is big, and purity is high, oxygen content is low, meets requirement of the target to material purity and consistency, and then greatly reduce tantalum and tantalum alloy target cost.
Description
Technical field
The present invention relates to nonferrous materials technical fields, more particularly to a kind of preparation side of the high-purity tantalum powder of target-grade
Method.
Background technique
In the prior art, mainly based on the processing of tantalum ingot, powder metallurgic method is easy to get with it for the preparation of tantalum target
Even aplitic texture, save material, the advantages such as production efficiency height have become another main preparation methods of magnetic control spattering target
And research hotspot.
The tantalum powder used as tantalum target must have two important conditions: one is purity is very high, generally 4N with
On；Secondly particle is preferably full particle, apparent density is big, because casting aside the factor of texture, the density and tantalum target of tantalum target
Quality it is closely bound up, the quality of the more high then tantalum target of the density of tantalum target is better.
In view of These characteristics, in addition to some tantalum powders used as addition element, powder metallurgic method prepares tantalum target use
Best tantalum powder be electron bombardment powder.But this tantalum powder raw material production procedure is long, and cost of manufacture is expensive, so limit powder
Metallurgy prepares the further development of tantalum target.
Currently, providing the acquisition pattern of tantalum powder there are also some patented technologies, but respectively have excellent lack:
102517460 A of Chinese patent CN provides the method for purification and tantalum target of a kind of tantalum powder, and technique includes: to mention
For low-purity tantalum powder；Radio frequency heating purification is carried out to the low-purity tantalum powder.But this method is only realized to tantalum powder
The raising of last purity.
Chinese patent CN 102367568 A provide a kind of manufacture craft of high-purity tantalum target, and tantalum powder is uniformly mixed；It will
Mixed tantalum powder is packed into mold；Cold moudling and then vacuum heating-press sintering.It is electron bombardment powder or tradition used herein of tantalum powder
Three-dimensional connection porous tantalum powder.Targetedly corrective measure is not proposed to traditional tantalum powder preparation process.
102382993 A of Chinese patent CN provides a kind of preparation method of target-grade ultrahigh-purity metal, and this method is in wet process
Recrystallization technique is increased in metallurgy, effectively reduces the content of refractory metal impurity and radioactive element.This method is
Some new thinkings are had found in the wet process for producing potassium floutaramite to improve the purity of tantalum powder.
Patent US 6323055 describes a kind of method for preparing High-purity Tantalum, High-purity Tantalum production and high-purity tantalum spattering target.It should
Method includes that purification raw material then refines High-purity Tantalum.This method is also the processing laid particular emphasis in the wet process of potassium floutaramite.
In the prior art, there are also tantalum ingot is prepared using electron bombardment during powder metallurgic method prepares tantalum target, then
Powder processed is hydrogenated again.This method manufacturing cost is too high.
Summary of the invention
It is an object of the invention to overcome the defect of the above-mentioned prior art, a kind of reduction tantalum powder internal voids are provided, effectively
Improve tantalum powder apparent density and purity, and simple process, the preparation method of the high-purity tantalum powder of the low target-grade of production cost.
The technical solution taken to achieve the purpose of the present invention are as follows:
A kind of preparation method of the high-purity tantalum powder of target-grade, it is characterised in that its processing step are as follows: first by sodium reduction fluorine tantalum
The mixing block material pure water diafiltration of tantalum powder made from sour potassium and diluting salt, when the conductivity of diafiltration liquid is less than 5000us/cm
When, the material after diafiltration is poured into horizontal ball mill and carries out wet ball-milling, material is taken out later and carries out pickling, suction filtration and dry
To tantalum powder original powder, then by tantalum powder original powder through Overheating Treatment, drop oxygen processing, drop oxygen pickling, again drying and detection obtain target-grade
High-purity tantalum powder；
One of NaCl, KCl and KF that above-mentioned diluting salt refers to or any is several.
The time with pure water diafiltration is 12~20 hours.
When the wet ball-milling, in 1:2~5, the solid-to-liquid ratio control of material and pure water exists for the weight ratio control of material and ball
1:0.5~1.5, Ball-milling Time 4~8 hours.
The HNO that it is 5~15% with mass concentration that the pickling, which refers to,3, 1~5% H2O2With the mixed acid of 0.2~2%HF
Liquid 2~4h of pickling, it is rear to stand, then impregnate 1~3h.
The drying refers to 10~15h of drying under the conditions of vacuum, 100~150 DEG C.
The heat treatment refers to handles 0.5~3h under the conditions of 800~1000 DEG C of temperature first, is then to slowly warm up to
1400~1550 DEG C continue with 0.5~3h, 10~20 DEG C/min of heating rate.
The drop oxygen processing is that oxygen is dropped using magnesium, mixes magnesium 0.5~3% in the tantalum powder after heat treatment, then evacuates argon filling, rises
For temperature to 850~1000 DEG C, heat preservation carries out reduction 1~3 hour, the row of evacuation magnesium 1~3 hour.
It is described drop oxygen pickling refer to use mass concentration for 5~15% HNO3It is carried out with the mix acid liquor of 0.2~2%HF
It is stood after 2~4h of pickling, then impregnates 1~3h again.
The present invention passes through direct after washing the mixing bulk material water of tantalum powder made from sodium reduction potassium floutaramite and diluting salt
It is put into ball mill, while pure water is added and carries out wet ball-milling crushing, can be broken the original spongiform porous body of tantalum powder in this way
It is bad, porosity is reduced, the densification for becoming it by loose structure；The impurity such as K, the Na being mingled in porous body simultaneously are also released
Come, is removed by subsequent pickling process, improve the purity of tantalum powder.The preparation method work of the high-purity tantalum powder of target-grade of the invention
Skill is simple, and production cost is low, and the tantalum powder apparent density prepared by this method is big, and purity is high, oxygen content is low, meets target to material
Expect the requirement of purity and consistency, and then greatly reduces tantalum and tantalum alloy target cost.
Specific embodiment
It elaborates below with reference to example to a specific embodiment of the invention.It should be understood that example is to be used for
It illustrates the invention and not limiting the invention.The scope of the present invention is determined with core content according to claims.
The mixing block material of tantalum powder made from sodium reduction potassium floutaramite and dilution composition is mitigated into blocky (dilution first
Liquid refers to one or more of NaCl, KCl and KF), it first uses pure water diafiltration 12~20 hours, when the conductivity of diafiltration liquid is less than
When 5000us/cm, the material after diafiltration is poured into horizontal ball mill and carries out ball milling, the weight ratio control of material and ball 1:2~
5, the solid-to-liquid ratio control of material and pure water is between 1:0.5~1.5, and Ball-milling Time 4~8 hours.It then takes out material and carries out acid
Wash, acid washing conditions here be use mass concentration for 5~15% HNO3, 1~5% H2O2With the mixing of 0.2~2%HF
Acid solution progress 2~4h of pickling, rear standing, then 1~3h is impregnated, then plus pure water is rinsed, is filtered, dry under vacuum (100~
150 DEG C/10~15h) tantalum powder original powder can be obtained.The tantalum powder original powder will also by normal subsequent heat treatment (800~1000 DEG C/
0.5~3h-, 1400~1550 DEG C/0.5~3h, 10~20 DEG C/min of heating rate), drop oxygen (using magnesium drop oxygen, after heat treatment
Tantalum powder in mix magnesium 0.5~3%, then evacuate argon filling, be warming up to 850~1000 DEG C, heat preservation carries out reduction 1~3 hour, evacuates
Row's magnesium 1~3 hour), drop oxygen pickling, drying (acid washing conditions here be use mass concentration for 5~15% HNO3And 0.2-
The mix acid liquor of 2%HF is stood after carrying out 2~4h of pickling, then impregnates 1-3h, and then plus pure water is rinsed, filtered, and is dried under vacuum
Dry (100~150 DEG C/10~15h)), the processes such as detection, finally obtain and improve porosity, improve apparent density and into one
Step improves the high-purity tantalum powder of densification of purity.
Embodiment 1:
Using NaCl as diluting salt carry out sodium reduction tantalum powder preparation, after reduction first by after sodium reduction tantalum powder with
The mixing block material of diluting salt NaCl is added pure water diafiltration 10 hours, when the conductivity of diafiltration liquid is 3000us/cm, shows
Most salt in tantalum powder have removed, and the material after diafiltration is then poured into horizontal ball mill and carries out ball milling, material and ball
Weight ratio control is in 1:2.5, and the solid-to-liquid ratio control of material and pure water is in 1:0.8, and Ball-milling Time 5 hours.Then take out material into
Row pickling, acid solution group become the HNO of mass concentration 10%3, 2% H2O2, add 0.5%HF, stand after pickling 2h, then
1.5h is impregnated again, and then plus pure water rinsing, suction filtration filter, and tantalum powder original powder can be obtained by drying (120 DEG C/14h) under vacuum.The tantalum
Powder original powder (will also be adopted by normal subsequent heat treatment (1000 DEG C/2h-, 1450 DEG C/1h, 10 DEG C/min of heating rate), drop oxygen
Oxygen is dropped with magnesium, magnesium 0.8% is mixed in the tantalum powder after heat treatment, then evacuates argon filling, is warming up to 900 DEG C, it is small that heat preservation carries out reduction 3
When, the row's of evacuation magnesium 2 hours), drop oxygen pickling, (acid washing conditions here are the HNO3 that mass concentration is 8%, add for drying
Stood after 0.3%HF pickling 2h, then impregnate 1h again, then plus pure water rinsing, filter, under vacuum dry (100 DEG C/15h),
The processes such as detection, the high-purity tantalum powder of densification for finally obtaining and improving porosity, improve apparent density and further increase purity.
Embodiment 2:
Using KCl as diluting salt carry out sodium reduction tantalum powder preparation, after reduction first by after sodium reduction tantalum powder with
The mixing block material of diluting salt KCl is added pure water diafiltration 15 hours, when the conductivity of diafiltration liquid is 1500us/cm, shows
Most salt in tantalum powder have removed, and the material after diafiltration is then poured into horizontal ball mill and carries out ball milling, material and ball
Weight ratio control is in 1:4, and the solid-to-liquid ratio control of material and pure water is in 1:1, and Ball-milling Time 8 hours.It then takes out material and carries out acid
It washes, acid solution group becomes the HNO of mass concentration 8%3, 3% H2O2, along with being stood after 0.7%HF pickling 2.5h, then soak again
1h is steeped, then plus pure water rinsing, suction filtration filter, and tantalum powder original powder can be obtained by drying (150 DEG C/12h) under vacuum.The tantalum powder original powder
Also (magnesium is used by normal subsequent heat treatment (1000 DEG C/2h-, 1480 DEG C/1.5h, 15 DEG C/min of heating rate), drop oxygen
Oxygen to be dropped, magnesium 1.2% is mixed in the tantalum powder after heat treatment, then evacuates argon filling, is warming up to 920 DEG C, heat preservation carries out reductase 12 .5 hours,
The row's of evacuation magnesium 1.5 hours), drop oxygen pickling, (acid washing conditions here are the HNO3 that mass concentration is 10%, add for drying
It is stood after 0.5%HF pickling 1.5h, then impregnates 1h again, then plus pure water is rinsed, is filtered, dry under vacuum (100 DEG C/
15h), the processes such as detection, the densification for finally obtaining and improving porosity, improve apparent density and further increase purity are high-purity
Tantalum powder.
Embodiment 3:
The preparation that sodium reduction tantalum powder is carried out using the salt-mixture of KCl and NaCl as diluting salt, first by sodium after reduction
The mixing block material of tantalum powder and diluting salt KCl and NaCl after reduction is added pure water diafiltration 20 hours, when the conductance of diafiltration liquid
When rate is 1000us/cm, shows that most salt in tantalum powder have removed, the material after diafiltration is then poured into horizontal ball mill
Ball milling is carried out, the weight ratio control of material and ball is in 1:5, and in 1:1.5, Ball-milling Time 9 is small for the solid-to-liquid ratio control of material and pure water
When.It then takes out material and carries out pickling, acid solution group becomes the HNO of mass concentration 10%3, 2% H2O2, along with 0.5%HF acid
It is stood after washing 2h, then impregnates 1.5h again, then plus pure water rinsing, suction filtration filter, and dry (120 DEG C/14h) under vacuum
Obtain tantalum powder original powder.The tantalum powder original powder will also pass through normal subsequent heat treatment (1000 DEG C/2h-, 1450 DEG C/1h, heating rate 10
DEG C/min), drop oxygen (drops oxygen using magnesium, mixes magnesium 0.8% in the tantalum powder after heat treatment, then evacuate argon filling, be warming up to 900 DEG C, protect
Temperature carries out reduction 3 hours, the row's of evacuation magnesium 2 hours), drop oxygen pickling, (acid washing conditions here are that mass concentration is 8% for drying
HNO3, along with being stood after 0.3%HF pickling 2h, then impregnate 1h again, then plus pure water rinsing, filter, dry under vacuum
The processes such as (100 DEG C/15h), detection, finally obtain and improve porosity, improve apparent density and further increase purity
Fine and close high-purity tantalum powder.
Comparative example 4:
The preparation of sodium reduction tantalum powder is carried out using the salt-mixture of KCl and NaCl as diluting salt, after reduction also by sodium
The mixing block material of tantalum powder and diluting salt KCl and NaCl after original is added pure water diafiltration 20 hours, when the conductivity of diafiltration liquid
When for 1000us/cm.It then takes out material and carries out pickling, acid solution group becomes the HNO of mass concentration 10%3, 2% H2O2, again plus
It is stood after upper 0.5%HF pickling 2h, then impregnates 1.5h again, then plus pure water rinsing, suction filtration filter, and dry (120 under vacuum
DEG C/14h) tantalum powder original powder can be obtained.The tantalum powder original powder will also by normal subsequent heat treatment (1450 DEG C of 1000 DEG C/2h -/
1h, 10 DEG C/min of heating rate), drop oxygen (oxygen is dropped using magnesium, magnesium 0.8% is mixed in the tantalum powder after heat treatment, then evacuates argon filling,
Be warming up to 900 DEG C, heat preservation carries out reduction 3 hours, the row's of evacuation magnesium 2 hours), drop oxygen pickling, (acid washing conditions here are matter for drying
Measure concentration be 8% HNO3, along with being stood after 0.3%HF pickling 2h, then impregnate 1h again, then plus pure water rinsing, filter,
The processes such as (100 DEG C/15h), detection are dried under vacuum, finally obtain the tantalum powder of normal process.
Example 1, example 2, example 3, comparative example 4 are analyzed, as a result 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 the table, Fsss (μm) indicates that Fei Shi partial size, SBD (g/cc) indicate apparent density, and+80 (%) indicate to be greater than 80
Ratio shared by purpose tantalum powder, -400 (%) represent less than ratio shared by the tantalum powder of 400 mesh.
Example 1, example 2, example 3 porosity compared with comparative example 4 reduce as can be seen from Table 1, and apparent density has increase, carefully
Powder ratio (- 400 mesh) is significantly increased, and original porous structure is broken, and powder becomes finer and close.Meet target tantalum powder
Porosity is low, the higher feature of density.
Table 2: major impurity content (unit: ppm) in tantalum powder
The detection method of element all derives from GB/T 15076.8-2008, GB/T 15076.9- in tantalum powder in upper table
2008、GB/T 15076.12-2008、GB/T 15076.14-2008、GB/T 15076.15-2008、GB/T 15076.16-
2008, the national standards such as " tantalum niobium chemical analysis method ".
Example 1, example 2, example 3 oxygen, carbon, iron equal size compared with comparative example 4 have different degrees of drop as can be seen from Table 2
It is low, meet the high-purity feature of target tantalum powder.
Claims (5)
1. a kind of preparation method of the high-purity tantalum powder of target-grade, it is characterised in that its processing step are as follows: first by sodium reduction fluorotantalic acid
The mixing block material pure water diafiltration of tantalum powder made from potassium and diluting salt, when the conductivity of diafiltration liquid is less than 5000us/cm,
Material after diafiltration is poured into horizontal ball mill and carries out wet ball-milling, material progress pickling, suction filtration and drying is taken out later and obtains
Tantalum powder original powder, then by tantalum powder original powder through Overheating Treatment, drop oxygen processing, drop oxygen pickling, again drying and detection obtain target-grade height
Pure tantalum powder；
One of NaCl, KCl and KF that above-mentioned diluting salt refers to or any is several；
The heat treatment refers to handles 0.5~3h under the conditions of 800~1000 DEG C of temperature first, then it is to slowly warm up to 1400~
1550 DEG C continue with 0.5~3h, 10~20 DEG C/min of heating rate；
The drop oxygen processing is that oxygen is dropped using magnesium, mixes magnesium 0.5~3% in the tantalum powder after heat treatment, then evacuates argon filling, be warming up to
850 DEG C~1000 DEG C, heat preservation carries out reduction 1~3 hour, the row of evacuation magnesium 1~3 hour；
It is described drop oxygen pickling refer to use mass concentration for 5~15% HNO3With the mix acid liquor of 0.2~2%HF carry out pickling 2~
It is stood after 4h, then impregnates 1-3h again.
2. the preparation method of the high-purity tantalum powder of target-grade described in accordance with the claim 1, it is characterised in that described with pure water diafiltration
Time is 12~20 hours.
3. the preparation method of the high-purity tantalum powder of target-grade described in accordance with the claim 1, it is characterised in that when the wet ball-milling, object
The weight ratio of material and ball is controlled in 1:2~5, and in 1:0.5~1.5, Ball-milling Time 4~8 is small for the solid-to-liquid ratio control of material and pure water
When.
4. the preparation method of the high-purity tantalum powder of target-grade described in accordance with the claim 1, it is characterised in that the pickling, which refers to, uses matter
Measure the HNO that concentration is 5~15%3, 1~5% H2O2It is rear to stand with mix acid liquor 2~4h of pickling of 0.2~2%HF, then impregnate 1
~3h.
5. the preparation method of the high-purity tantalum powder of target-grade described in accordance with the claim 1, it is characterised in that the drying refers to true
It is empty, dry 10~15h under the conditions of 100~150 DEG C.
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| 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 |
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