CN111893325A - High-purity tantalum ingot and preparation method thereof - Google Patents
High-purity tantalum ingot and preparation method thereof Download PDFInfo
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000003723 Smelting Methods 0.000 claims abstract description 78
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 238000010894 electron beam technology Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 230000007547 defect Effects 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 238000000462 isostatic pressing Methods 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 239000013077 target material Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 238000005266 casting Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
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Abstract
The invention relates to a high-purity tantalum ingot and a preparation method thereof. The method is characterized by comprising the following steps: (1) forming tantalum powder with low content of high-melting-point metal impurities; (2) sintering at high temperature under vacuum to obtain tantalum rods, tantalum strips or tantalum blocks, and preparing a smelting electrode for vacuum electron beam smelting by adopting tantalum wires with the same purity; (3) smelting at least twice by using a vacuum electron beam smelting furnace, wherein the first smelting is required to adopt a horizontal feeding mode or a vertical feeding mode, and the second smelting or the later smelting adopts a vertical feeding mode; when the second or later electrode smelting is carried out, the rotation of the electrode is required, and the rotation speed is controlled to be 0.3-0.8 r/min. Through the control of the smelting process, the smelted tantalum cast ingot has high purity, particularly lower interstitial impurity element C, O, N, H, low hardness of the cast ingot and less defects of air holes, looseness, shrinkage cavities and the like, and is suitable for preparing high-end processing materials such as tantalum target materials and the like by pressure processing.
Description
Technical Field
The invention relates to a high-purity tantalum ingot and a preparation method thereof.
Background
Tantalum is an important metal material in industry, has high melting point and good corrosion resistance, is applied to wide fields, is mainly used as tantalum powder and tantalum wires of a sintering anode of an electrolytic capacitor, and is used for manufacturing structural materials such as a heating body and an insulating layer of a high-temperature vacuum furnace, chemical anti-corrosion materials, high-temperature alloy, hard alloy and super alloy. Tantalum metal has excellent dielectric property, chemical stability, thermal conductivity and special corrosion resistance, so that the target material can be used as an electronic material, a sputtering film material and a corrosion-resistant material and is widely applied to the aspects of microelectronic industry, flat panel displays, optical disks, magnetic head disks and the like. The application of high-purity refractory metal Ta as a wiring material, a sputtering target material, and the like to a large-scale integrated circuit has attracted attention from various countries, and is considered to be a microelectronic material with great future.
The preparation technology of the target material can be divided into two technical routes of smelting and thermal mechanical treatment and powder sintering and thermal mechanical treatment according to the main processing process, wherein the preparation of the tantalum target material mainly adopts the smelting and thermal mechanical treatment method to carry out the microstructure control and blank forming on the tantalum cast ingot by the thermal mechanical treatment technologies such as forging, rolling and thermal treatment. The high-purity tantalum foil is used for manufacturing a shell of a tantalum capacitor, is used for packaging the full-tantalum capacitor, is mainly applied to high-reliability military tantalum capacitors, and requires the stamping performance and the higher purity of the tantalum foil, and the defects of microcrack prevention and the like of the tantalum foil are the primary requirements. At present, tantalum ingots in different forms are mainly produced by taking tantalum as a smelting electrode and smelting by one or a combination of vacuum consumable arc, vacuum electron beam, vacuum plasma beam and plasma arc.
Regardless of the melting method, the casting quality of the ingot is the most critical. The production of high-quality tantalum ingots is the primary link in metal pressure processing production and is also an indispensable component. It not only supplies raw material-ingot necessary for processing part, but also influences the quality and technological performance of the processed product to a great extent. Therefore, the fusion casting and ingot casting production provides the high-quality ingot casting meeting the pressure processing production requirement. The casting task mainly comprises the following aspects of 1) obtaining metal with uniform chemical components and purity meeting the use requirement, 2) casting the metal into an ingot with the shape and the size suitable for pressure processing, wherein the ingot has small processing resistance and is suitable for deformation processing, 3) controlling the crystal structure, the shape and the distribution of the ingot, 4) the inner part of the ingot has no structural defects such as air holes, cracks and the like, and the crystal structure of the ingot is fine and can reach the theoretical density.
Disclosure of Invention
The invention aims to provide a large-size, high-purity, low-defect and low-hardness high-purity metal tantalum cast ingot which is suitable for preparing a tantalum target material for sputtering and other tantalum processing materials with special purposes.
A high-purity tantalum ingot is composed of Ta and impurities, wherein the Ta is more than or equal to 99.999% in percentage by mass.
Wherein Nb in the impurities is less than or equal to 2ppm, W is less than or equal to 1ppm, Mo is less than or equal to 1ppm, U is less than or equal to 0.001ppm, Th is less than or equal to 0.001ppm, S is less than 0.015ppm, Si is less than or equal to 0.08ppm, C is less than or equal to 10ppm, O is less than or equal to 15ppm, N is less than or equal to 15ppm, H is less than or equal to 2ppm, and other inevitable impurities, wherein the total amount of metal impurities is not more than 10ppm except.
The hardness HV/9.8N of the cast ingot is less than or equal to 85.
Wherein the ingot is detected by ultrasonic flaw detection, the control interval is more than 50mm, and the wave height is more than
Equivalent weight, defect rate less than or equal to 1 percent
In which the casting is carried outThe density of the ingot is 16.5-16.6 g/cm3。
The preparation method of the high-purity tantalum ingot is characterized by comprising the following steps:
(1) forming tantalum powder with low content of high-melting-point metal impurities;
(2) sintering at high temperature under vacuum to obtain tantalum rods, tantalum strips or tantalum blocks, and preparing a smelting electrode for vacuum electron beam smelting by adopting tantalum wires with the same purity;
(3) smelting at least twice by using a vacuum electron beam smelting furnace, wherein the first smelting is required to adopt a horizontal feeding mode or a vertical feeding mode, and the second smelting or the later smelting adopts a vertical feeding mode;
when the second or later electrode smelting is carried out, the rotation of the electrode is required, and the rotation speed is controlled to be 0.3-0.8 r/min.
And (3) operating the electron beams in an interval scanning mode to ensure the melting of the melting electrode and the maintenance of a molten pool, wherein the scanning track of the electron beams is controlled by taking the center of the crucible as an origin, the scanning tracks and the scanning residence time of different sizes are controlled, the maximum scanning track of a single gun is 9/10 of the radius of the crucible, and the maximum scanning track is sequentially decreased according to 1/10 of the radius of the crucible to form 8 scanning tracks in the molten pool, wherein the scanning residence time of the maximum scanning track is 100-140 ms.
The smelting electrode for vacuum electron beam smelting prepared in the step (2) specifically adopts a binding or welding mode.
In the tantalum powder with low content of high-melting-point metal impurities in the step (1), Nb is less than or equal to 0.001 percent, W is less than or equal to 0.0005 percent, and Mo is less than or equal to 0.0005 percent according to weight percentage.
The forming in the step (1) specifically adopts isostatic pressing forming or compression molding forming, and the forming pressure is controlled to be more than or equal to 200 MPa.
In the step (2), the high-temperature sintering temperature is controlled to be more than or equal to 1800 ℃, the heat preservation time is more than or equal to 6 hours, and the relative density after sintering is more than or equal to 70 percent.
The vacuum degree of the smelting chamber is required to be more than or equal to 1.0 multiplied by 10 in the smelting process of the step (3)-2Pa, the specific electric energy during smelting, namely the ratio of smelting power to smelting speed is more than or equal to 4, and the cooling water temperature during smelting is controlledAnd cooling the tantalum ingot formed after smelting in a vacuum cooling chamber for more than or equal to 6 hours at the temperature of between 20 and 30 ℃.
The high-purity tantalum ingot has the following advantages: through the control of the smelting process, the smelted tantalum cast ingot has high purity, particularly lower interstitial impurity element C, O, N, H, low hardness of the cast ingot and less defects of air holes, looseness, shrinkage cavities and the like, and is suitable for preparing high-end processing materials such as tantalum target materials and the like by pressure processing.
Drawings
FIG. 1 is a flow chart of a production process of a high-purity tantalum ingot;
FIG. 2 is a schematic diagram showing electron beam scanning trajectory of a high-purity tantalum ingot molten pool.
Detailed Description
The invention is further illustrated with reference to the figures and examples.
The following examples were produced according to the process flow of FIG. 1.
Example 1:
weighing 500Kg of tantalum powder with low content of high-melting-point metal impurities, meeting the requirement of FTa-1 in tantalum powder industry standard YS/T259-2012, wherein the tantalum powder is provided by Ningxia Oriental tantalum industry Co., Ltd, filling the tantalum powder into a rubber sleeve, sealing, and carrying out compression molding in a cold isostatic press at a molding pressure of 200 MPa.
Sintering the formed tantalum rod at high temperature in vacuum, wherein the sintering process is shown in table 1. Binding sintered tantalum rods with tantalum wires with the same purity to prepare smelting electrodes, wherein a smelting crucible is adopted
The primary smelting adopts a horizontal feeding smelting mode, the smelting power is 500kw, the smelting speed is 85Kg/h, the secondary smelting adopts a vertical feeding mode, the smelting power is 520kw, the smelting speed is 80Kg/h, and the vacuum degree of a smelting chamber required in the smelting process is more than or equal to 1.0 multiplied by 10-2Pa. The cooling water temperature during smelting is controlled at 26 ℃, and the tantalum ingot formed after smelting is cooled in a vacuum cooling chamber for more than 6 hours.
When the secondary electrode smelting is carried out, the electrode is required to rotate, the rotating speed is 0.6r/min, and the scanning track control of the smelting is shown in a table 2.
In particular high purityThe tantalum ingot analysis results are shown in tables 3 and 4. Flaw detection is carried out according to the ultrasonic flaw detection and quality grading method of the steel castings, and the equivalent value of the flaw is
The defect continuous length is less than or equal to 50mm, and the defect rate can be detected to be less than 1%.
TABLE 1 sintering Process of tantalum bars
| Step (ii) of | |
| 1 | Room temperature → 700 ℃ -800 ℃, 2h rising, and heat preservation for |
| 2 | Rising the temperature to 700-800 → 1600-1700 ℃, keeping the temperature for 3h. |
| 3 | 1600-1700 ℃ to → 1900 ℃ and rising to 3h for heat preservation for |
| 4 | Vacuum cooling or argon filling cooling to room temperature in case of power failure |
TABLE 2 melting scan trajectory control
TABLE 3 analysis of impurities in high purity tantalum ingot
(the high-purity tantalum ingot has lower interstitial impurity elements and low hardness, is easy to process high-end products such as target materials and the like, and the low impurity elements can effectively prevent the target materials from abnormal discharge in the sputtering process so as to ensure the quality of sputtered films)
TABLE 4 GDMS analysis results of high purity tantalum ingots
| Determination of elements | Measurement result/ppm (wt) | Determination of elements | Measurement result/ppm (wt) |
| Li | ＜0.003 | Pd | ＜0.005 |
| Be | ＜0.003 | Ag | ＜0.005 |
| B | ＜0.005 | Cd | ＜0.005 |
| C | -- | In | ＜0.005 |
| N | -- | Sn | ＜0.005 |
| O | -- | Sb | ＜0.005 |
| F | ＜0.5 | Te | ＜0.005 |
| Na | ＜0.005 | I | ＜0.005 |
| Mg | ＜0.005 | Cs | ＜0.005 |
| Al | ＜0.005 | Ba | ＜0.005 |
| Si | ＜0.06 | La | ＜0.005 |
| P | ＜0.005 | Ce | ＜0.005 |
| S | ＜0.015 | Pr | ＜0.005 |
| Cl | ＜0.03 | Nd | ＜0.005 |
| K | 0.006 | Sm | ＜0.005 |
| Ca | ＜0.005 | Eu | ＜0.005 |
| Sc | ＜0.003 | Gd | ＜0.005 |
| Ti | ＜0.005 | Tb | ＜0.005 |
| V | ＜0.003 | Dy | ＜0.005 |
| Cr | ＜0.005 | Ho | ＜0.005 |
| Mn | ＜0.003 | Er | ＜0.005 |
| Fe | ＜0.005 | Tm | ＜0.005 |
| Co | ＜0.003 | Yb | ＜0.005 |
| Ni | ＜0.005 | Lu | ＜0.005 |
| Cu | ＜0.005 | Hf | ＜0.005 |
| Zn | ＜0.005 | Ta | Matrix |
| Ga | ＜0.005 | W | 0.023 |
| Ge | ＜0.005 | Re | ＜0.005 |
| As | ＜0.005 | Os | ＜0.005 |
| Se | ＜0.03 | Ir | ＜0.005 |
| Br | ＜0.005 | Pt | ＜0.05 |
| Rb | ＜0.005 | Au | ＜0.05 |
| Sr | ＜0.005 | Hg | ＜0.005 |
| Y | ＜0.003 | Tl | ＜0.005 |
| Zr | ＜0.005 | Pb | ＜0.005 |
| Nb | 0.44 | Bi | ＜0.01 |
| Mo | 0.015 | Th | ＜0.001 |
| Ru | ＜0.005 | U | ＜0.001 |
| Rh | ＜0.005 |
(the purity of the tantalum cast ingot reaches more than 5N, most elements reach the lower limit of a GDMS analysis method, the requirement of the high-purity tantalum cast ingot for the sputtering target material is completely met, and necessary conditions are provided for the preparation of the high-purity tantalum target material)
Example 2:
250Kg of tantalum powder with low content of high-melting-point metal impurities is weighed to meet the requirement of FTa-1 in the tantalum powder industry standard YS/T259-2012. (tantalum powder is provided by Ningxia Oriental tantalum industry Co., Ltd.) tantalum powder is put into a steel die-pressing strip-shaped appliance, and is pressed and formed by adopting an oil pressure device, the forming pressure is 180Mpa, and the formed strip-shaped object can move without breaking.
And (3) sintering the formed tantalum strip at high temperature in vacuum, wherein the sintering process is shown in table 1. Binding the sintered tantalum strips with tantalum wires with the same purity to prepare a smelting electrode, wherein a smelting crucible is adopted
The primary smelting adopts a horizontal feeding smelting mode, the smelting power is 420kw, the smelting speed is 80Kg/h, the secondary smelting adopts a vertical feeding mode, the smelting power is 440kw, the smelting speed is 75Kg/h, and the vacuum degree of a smelting chamber required in the smelting process is more than or equal to 1.0 multiplied by 10-2Pa. The temperature of input cooling water during smelting is controlled at 26 ℃ (the embodiment is similar to a specific experimental record, wherein the data should be specific numerical values, please modify), and tantalum ingots formed after smelting are cooled in a vacuum cooling chamber for more than 5 h.
TABLE 5 melting scan trajectory control
TABLE 6 analysis results of impurities in high purity tantalum ingot gas
When the secondary electrode smelting is carried out, the electrode is required to rotate, the rotating speed is 0.5r/min, and the scanning track control of the smelting is shown in a table 5.
TABLE 7 GDMS analysis results of high purity tantalum ingots
| Determination of elements | Measurement result/ppm (wt) | Determination of elements | Measurement result/ppm (wt) |
| Li | ＜0.001 | Pd | ＜0.005 |
| Be | ＜0.003 | Ag | ＜0.005 |
| B | ＜0.005 | Cd | ＜0.005 |
| C | -- | In | ＜0.005 |
| N | -- | Sn | ＜0.005 |
| O | -- | Sb | ＜0.005 |
| F | ＜0.5 | Te | ＜0.005 |
| Na | 0.008 | I | ＜0.005 |
| Mg | ＜0.005 | Cs | ＜0.005 |
| Al | ＜0.005 | Ba | ＜0.005 |
| Si | ＜0.06 | La | ＜0.005 |
| P | ＜0.005 | Ce | ＜0.005 |
| S | ＜0.015 | Pr | ＜0.005 |
| Cl | 0.044 | Nd | ＜0.005 |
| K | 0.012 | Sm | ＜0.005 |
| Ca | ＜0.005 | Eu | ＜0.005 |
| Sc | ＜0.003 | Gd | ＜0.005 |
| Ti | ＜0.005 | Tb | ＜0.005 |
| V | ＜0.001 | Dy | ＜0.005 |
| Cr | ＜0.005 | Ho | ＜0.005 |
| Mn | ＜0.001 | Er | ＜0.005 |
| Fe | ＜0.005 | Tm | ＜0.005 |
| Co | ＜0.003 | Yb | ＜0.005 |
| Ni | ＜0.005 | Lu | ＜0.005 |
| Cu | 0.021 | Hf | ＜0.005 |
| Zn | ＜0.005 | Ta | Matrix |
| Ga | ＜0.005 | W | 0.83 |
| Ge | ＜0.005 | Re | ＜0.005 |
| As | ＜0.005 | Os | ＜0.005 |
| Se | ＜0.03 | Ir | ＜0.005 |
| Br | ＜0.005 | Pt | ＜0.05 |
| Rb | ＜0.005 | Au | ＜0.05 |
| Sr | ＜0.005 | Hg | ＜0.005 |
| Y | ＜0.003 | Tl | ＜0.005 |
| Zr | ＜0.005 | Pb | ＜0.005 |
| Nb | 0.82 | Bi | ＜0.01 |
| Mo | 0.18 | Th | ＜0.001 |
| Ru | ＜0.005 | U | ＜0.001 |
| Rh | ＜0.005 |
Specific analysis results of the high purity tantalum ingots are shown in tables 6 and 7. Flaw detection is carried out according to the ultrasonic flaw detection and quality grading method of the steel castings, and the equivalent value of the flaw is
The defect continuous length is less than or equal to 50mm, and the defect rate can be detected to be less than 1%.
Claims (12)
1. A high-purity tantalum ingot is composed of Ta and impurities, wherein the Ta is more than or equal to 99.999% in percentage by mass.
2. The high purity tantalum ingot of claim 1, wherein: wherein Nb in the impurities is less than or equal to 2ppm, W is less than or equal to 1ppm, Mo is less than or equal to 1ppm, U is less than or equal to 0.001ppm, Th is less than or equal to 0.001ppm, S is less than 0.015ppm, Si is less than or equal to 0.08ppm, C is less than or equal to 10ppm, O is less than or equal to 15ppm, N is less than or equal to 15ppm, H is less than or equal to 2ppm, and other inevitable impurities, wherein the total amount of metal impurities is not more than 10ppm except.
3. The high purity tantalum ingot of claim 1, wherein: the hardness HV/9.8N of the cast ingot is less than or equal to 85.
4. The high purity tantalum ingot of claim 1, wherein: wherein the ingot is detected by ultrasonic flaw detection, the control interval is more than 50mm, and the wave height is more than
Equivalent weight, and defect rate less than or equal to 1 percent.
5. The high purity tantalum ingot of claim 1, wherein: wherein the density of the cast ingot is 16.5-16.6 g/cm3。
6. The preparation method of the high-purity tantalum ingot is characterized by comprising the following steps:
(1) forming tantalum powder with low content of high-melting-point metal impurities;
(2) sintering at high temperature under vacuum to obtain tantalum rods, tantalum strips or tantalum blocks, and preparing a smelting electrode for vacuum electron beam smelting by adopting tantalum wires with the same purity;
(3) smelting at least twice by using a vacuum electron beam smelting furnace, wherein the first smelting is required to adopt a horizontal feeding mode or a vertical feeding mode, and the second smelting or the later smelting adopts a vertical feeding mode;
when the second or later electrode smelting is carried out, the rotation of the electrode is required, and the rotation speed is controlled to be 0.3-0.8 r/min.
7. The method for preparing high purity tantalum ingots according to claim 6, wherein: and (3) operating the electron beams in an interval scanning mode to ensure the melting of the melting electrode and the maintenance of a molten pool, wherein the scanning track of the electron beams is controlled by taking the center of the crucible as an origin, the scanning tracks and the scanning residence time of different sizes are controlled, the maximum scanning track of a single gun is 9/10 of the radius of the crucible, and the maximum scanning track is sequentially decreased according to 1/10 of the radius of the crucible to form 8 scanning tracks in the molten pool, wherein the scanning residence time of the maximum scanning track is 100-140 ms.
8. The method for preparing high purity tantalum ingots according to claim 6, wherein: the smelting electrode for vacuum electron beam smelting prepared in the step (2) specifically adopts a binding or welding mode.
9. The method for preparing high purity tantalum ingots according to claim 6, wherein: in the tantalum powder with low content of high-melting-point metal impurities in the step (1), Nb is less than or equal to 0.001 percent, W is less than or equal to 0.0005 percent, and Mo is less than or equal to 0.0005 percent according to weight percentage.
10. The method for preparing high purity tantalum ingots according to claim 6, wherein: the forming in the step (1) specifically adopts isostatic pressing forming or compression molding forming, and the forming pressure is controlled to be more than or equal to 200 MPa.
11. The method for preparing high purity tantalum ingots according to claim 6, wherein: in the step (2), the high-temperature sintering temperature is controlled to be more than or equal to 1800 ℃, the sintering heat preservation time is more than or equal to 6 hours, and the relative density after sintering is more than or equal to 70 percent.
12. The method for preparing high purity tantalum ingots according to claim 6, wherein: the vacuum degree of the smelting chamber is required to be more than or equal to 1.0 multiplied by 10 in the smelting process of the step (3)-2Pa, the specific electric energy during smelting, namely the ratio of smelting power to smelting speed, is not less than 4, the cooling water temperature during smelting is controlled at 20-30 ℃, and tantalum ingots formed after smelting are cooled in a vacuum cooling chamber for not less than 6 hours.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911396875 | 2019-12-30 | ||
| CN2019113968757 | 2019-12-30 |
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Cited By (5)
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| CN113005299A (en) * | 2021-02-23 | 2021-06-22 | 宁夏东方钽业股份有限公司 | Tantalum metal biological implant and preparation method thereof |
| CN114892028A (en) * | 2022-04-11 | 2022-08-12 | 同创(丽水)特种材料有限公司 | Recovery method of target ring piece |
| CN115572844A (en) * | 2022-10-27 | 2023-01-06 | 先导薄膜材料有限公司 | Method for recovering tantalum from tantalum residue target |
| CN116751979A (en) * | 2023-06-21 | 2023-09-15 | 同创(丽水)特种材料有限公司 | High-purity tantalum ingot 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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| CN116751979A (en) * | 2023-06-21 | 2023-09-15 | 同创(丽水)特种材料有限公司 | High-purity tantalum ingot and preparation method thereof |
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