CN107619955A - The high-purity tantalum foil preparation methods of OLED - Google Patents
The high-purity tantalum foil preparation methods of OLED Download PDFInfo
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- CN107619955A CN107619955A CN201710863948.3A CN201710863948A CN107619955A CN 107619955 A CN107619955 A CN 107619955A CN 201710863948 A CN201710863948 A CN 201710863948A CN 107619955 A CN107619955 A CN 107619955A
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Abstract
The invention belongs to organic electric exciting light-emitting diode (OLED) manufacturing field, it is related to the evaporation boat used during deposit metal electrodes, and in particular to the high-purity tantalum foil evaporation boat preparation methods of OLED, including：Stock, shove charge, melting once, vacuum cooled, secondary smelting, split rolling method, the pickling of tantalum ingot, stock, vacuum annealing heat treatment and rolling.By using electronic torch melting, area smelting refinement, electromagnetic field purification and accurate control speed of melting, time, ensure that tantalum foil impurity content is few, purity is high；High-power milling train cogging by rolling mill practice and directly is carried out, technological process is simplified, improves operating efficiency, and makes that the tantalum foil fault of construction that processes is few, grainiess is careful, the uniformity is high, sheet material interior mechanics performance isotropism is high.
Description
Technical field
The invention belongs to organic electric exciting light-emitting diode (OLED) manufacturing field, is related to OLED with high-purity tantalum foil preparation side
Method.
Background technology
Organic electric exciting light-emitting diode (OLED) is due to being provided simultaneously with self-luminous, being not required to backlight, contrast height, thickness
It is thin, visual angle is wide, reaction speed is fast, available for flexibility panel, the excellent spy such as use temperature range is wide, construction and processing procedure are simpler
Property, it is considered to be the follow-on emerging application technology of flat-panel screens.OLED is by one layer of thin, transparent tool characteristic of semiconductor
Indium tin oxide (ITO) be connected with electrode anode, formed anode；Layer of metal negative electrode, along with the anode and metal are cloudy
The sandwich structure that luminescent layer between pole is bundled into.Wherein deposit metal electrodes when use evaporation boat made of tantalum foil material
Effect is best.
Organic electric exciting light-emitting diode device can be divided into two kinds by luminescent material：Small molecule OLED and macromolecule OLED (
Can be described as PLED), their Main Differences show that the preparation technology of device is different：Small molecule devices are mainly steamed using Vacuum Heat
Hair technique, macromolecule device then use rotary coating or ink-jetting process.The vacuum evaporation process OLED of organic film needs
Multilayer organic film, the relationship between quality of film to device quality and life-span are deposited in high-vacuum chamber.In high-vacuum chamber
Evaporation boat provided with multiple placement organic materials, heating evaporation boat evaporation organic material, and controlled using quartz oscillator
Film is thick.
For supporting whole OLED basic unit (transparent plastic, glass, metal foil), particularly foldable OLED basic units are by soft
The good metal foil of toughness or plastics are made.High-purity tantalum foil basic unit have surface-brightening, flawless, without peeling, unfolded, without bright
The advantages that aobvious oxidation and free from admixture press-in defect, but its processing difficulties, low production efficiency, product quality cannot ensure, it is difficult
With volume production.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of impurity content in strict conformity with standard, structure
The high-purity tantalum foil systems of the OLED that defect is few, grainiess is careful, the uniformity is high, sheet material interior mechanics performance isotropism is high
Preparation Method.
The technical proposal for solving the technical problem of the invention is：
The high-purity tantalum foil preparation methods of OLED, it is characterised in that comprise the following steps：
Step 1 is stocked up：Select niobium, W content low, the tantalum bar of purity >=99.8%；
Step 2 shove charge：Clearing furnace, ensure to clear up reactor without the debris that drops in vacuum chamber, avoid polluting, keep high
Pure environment, tantalum bar tie up material shove charge；
Step 3 melting once：Using electron beam furnace melting, melting is started to warm up in burner hearth vacuum≤0.006pa, is tieed up
Hold smelting temperature >=3050 DEG C, according to melting tantalum bar quality how much, control smelting time, refining speed be maintained at≤45kg/h, and
The accurate distribution of appropriateness manipulation electron beam, ensures fully to melt tantalum bar；
Step 4 vacuum cooled：The High-purity Tantalum ingot that melting is completed, 8h~12h is cooled down under vacuum conditions and is come out of the stove；
Step 5 secondary smelting：Repeat step 3；
Step 6 split rolling method：Using 2000 tons of 1.2 meters of reversible cold, hot two-purpose milling trains, using the method for tandem rolling, and
The drafts rolled each time is controlled between 12% to 18%；
Step 7 tantalum ingot pickling：Acidwash solution formula uses the mixed solution of hydrochloric acid and hydrofluoric acid, and the concentration of hydrochloric acid is
25wt% to 35wt%, the concentration of hydrofluoric acid is 40wt% to 50wt%, soaks tantalum ingot 5min in Acidwash solution under normal temperature and arrives
15min；
Step 8 is stocked up：Stocked up with 800mm milling trains to 0.5mm-0.8mm；
Step 9 vacuum annealing is heat-treated：Control vacuum 0.001Pa, 900 DEG C to 1300 DEG C of maximum temperature, in the highest temperature
Lower soaking time 90min to the 120min of degree；
Step 10 rolls：With 300mm band and strip rolling mills, it is 0.05mm High-purity Tantalum foils to produce thickness.
Further, as a further improvement on the present invention, it is characterised in that：The step 3 in metallic crystal process also
Additional electromagnetic field purifies, and controls magnetic field intensity 4800-600A/m.
Further, as a further improvement on the present invention, it is characterised in that：Electron beam furnace melting in the step 3
For zone refining, at a temperature of 2900 DEG C -3500 DEG C, the long and narrow material ingot shapes of local electronic Shu Jiare are into a narrow melting
Area, and electron beam is heated by mobile, this narrow melting zone is slowly moved along material ingot in certain direction, using impurity in solid phase
With liquid phase homostasis concentration difference, during being repeatedly melted and solidifying, impurity segregation is set to be able into solid phase or liquid phase
Remove or redistribute.
Further, as a further improvement on the present invention, it is characterised in that the melting zone uses resistance heating, and
By mobile adding thermal resistance, this narrow melting zone is set slowly to be moved along material ingot in certain direction, using impurity in solid phase and liquid phase
Homostasis concentration difference, during being repeatedly melted and solidifying, make impurity segregation be able to remove into solid phase or liquid phase or
Redistribution.
Further, as a further improvement on the present invention, it is characterised in that the melting zone uses sensing heating, and
By mobile heat induced, the narrow melting zone is set slowly to be moved along material ingot in certain direction, using impurity in solid phase and liquid
Identical equilibrium concentration difference, during being repeatedly melted and solidifying, impurity segregation is set to be removed into solid phase or liquid phase
Or redistribution.
Further, as a further improvement on the present invention, it is characterised in that：Secondary smelting repeats to walk in the step 5
Rapid 3 number is 1 time, 2 times or 3 times.
Further, as a further improvement on the present invention, it is characterised in that：In the step 6 during tandem rolling
Add intermediate annealing process.
Further, as a further improvement on the present invention, it is characterised in that：The first of tandem rolling in the step 6
Secondary rolling direction is vertical with second of rolling direction.
Further, as a further improvement on the present invention, it is characterised in that：The first of tandem rolling in the step 6
Secondary rolling direction is with second of rolling direction into 15 ° to 85 °.
By above technical scheme, the technique effect that the present invention realizes is：
1. tantalum foil impurity content is few, purity is high, specifically, is realized from the following aspects：
1) electronic torch melting is used：(2600-3000 DEG C) vacuum melting refers to remove Gases In Metals under vacuum
The process of impurity, actually reduce the solubility of gaseous impurity in a metal.According to Xi Weici laws, diatomic gas under constant temperature
The square root of body solubility in a metal and partial pressure is directly proportional.Therefore the vacuum of system is improved, just equivalent to reduction
The partial pressure of gas, the solubility of gas in a metal can be also reduced, and the portion gas impurity more than solubility will be from gold
Escape and remove in category.
Under the conditions of high vacuum (2.5-6 μ Pa), moisture drastically volatilizees at 100-200 DEG C, 600-700 DEG C of hydride decomposition
Effusion, alkali metal and its compound are volatilized at a temperature of 1100-1600 DEG C, and most of iron, nickel, chromium etc. are with low melting point oxide shape
State is volatilized, nitrogen volatilization effusion at 2300 DEG C, contrast hydrogen, the nitrogen oxygen big to metal affinity, then with add carbon deoxidation ([C]+[O]=
CO ↑) and above foreign metal low oxide MeON mode remove.
2) area smelting refinement is used：(2900-3150 DEG C) zone refining is a kind of method that depth is purified metals, in fact
Matter is into a narrow melting zone by the long and narrow material ingot shape of local heating, and mobile heating makes this narrow melting zone by certain side
Slowly moved to along material ingot, using impurity in solid phase and liquid phase homostasis concentration difference, during being repeatedly melted and solidifying,
Impurity just segregates in solid phase or liquid phase and is able to remove or redistributes；Melting zone typically uses resistance heating, sensing heating or
Electron beam heats.
3) purified using electromagnetic field：The depth purification high-melting-point gold under electromagnetic field (magnetic field intensity 4800-6000A/m) effect
The technology of category is used more and more.Electromagnetic field is not limited to the stirring action to molten metal, and more important is under electromagnetic field
Molten metal can be made to obtain being uniformly distributed for fault of construction, and refined grain structure in crystallization process.Crystallized in multiphase system
When, it can separate out the second phase orientation using electromagnetic field, electromagnetic field plays energy supporting role and stirring action, utilizes the evaporation of impurity
The second phase (oxide, carbide etc.), which is walked, with drift carrys out purified metal.
4) according to the number selection speed of melting of material, time, in fusion process by controlling the accurate scanning of electron beam,
Removed with the volatilization of the purity and impurity of maximum efficiency control metal.
In the case of from high-purity tantalum foil, ensure smelting temperature >=3050 DEG C, low-melting-point metal impurity content is respectively less than
1ppm, the impurity contents such as Nb, W are effectively reduced, so as to obtain high-purity nickel ingot.When melting vacuum is≤1 × 10-2pa
It can ensure that gaseous impurity content is very low, C, N, O are respectively less than 50ppm；Multiple smelting metal tantalum ingot purity can be higher.The present embodiment
Impurity analysis result is shown in《Impurity analysis result GDMS results》, as seen from the table, Nb, W content control are comparatively ideal in tantalum ingot
Value, other constituent contents also control more significant, so as to ensure that tantalum ingot purity >=99.99%.
2. tantalum foil fault of construction is few, grainiess is careful, the uniformity is high, sheet material interior mechanics performance isotropism
Height, specifically, realized from the following aspects：
1) rolling mill practice：High-performance OLED has high want with high-purity tantalum foil to metal purity, grain size and uniformity
Ask, this technique is since strict control into factory's raw material metal impurity content, in tantalum foil forms process, using large deformation
Tandem rolling and intermediate annealing process are measured, optimizes rolling technological parameter and annealing temperature, ensures the mechanical property of sheet material respectively to same
Property, uniform, tiny grain structure is obtained after annealing.
2) hammer cogging is not used, high-power milling train cogging is directly carried out, simplifies technological process, improves work effect
Rate.
By this project implementation, it can produce and meet the high-purity tantalum foils of OLED, its size can reach：0.05*280*
Lmm, purity reach 99.99%.
Embodiment
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of impurity content in strict conformity with standard, structure
The high-purity tantalum foil systems of the OLED that defect is few, grainiess is careful, the uniformity is high, sheet material interior mechanics performance isotropism is high
Preparation Method.
The technical proposal for solving the technical problem of the invention is：
The high-purity tantalum foil preparation methods of OLED, it is characterised in that comprise the following steps：
Step 1 is stocked up：Select niobium, W content low, the tantalum bar of purity >=99.8%；
Step 2 shove charge：Clearing furnace, ensure to clear up reactor without the debris that drops in vacuum chamber, avoid polluting, keep high
Pure environment, tantalum bar tie up material shove charge；
Step 3 melting once：Using electron beam furnace melting, melting is started to warm up in burner hearth vacuum≤0.006pa, is tieed up
Hold smelting temperature >=3050 DEG C, according to melting tantalum bar quality how much, control smelting time, refining speed be maintained at≤45kg/h, and
The accurate distribution of appropriateness manipulation electron beam, ensures fully to melt tantalum bar；
Step 4 vacuum cooled：The High-purity Tantalum ingot that melting is completed, 8h~12h is cooled down under vacuum conditions and is come out of the stove；
Step 5 secondary smelting：Repeat step 3；
Step 6 split rolling method：Using 2000 tons of 1.2 meters of reversible cold, hot two-purpose milling trains, using the method for tandem rolling, and
The drafts rolled each time is controlled between 12% to 18%；
Step 7 tantalum ingot pickling：Acidwash solution formula uses the mixed solution of hydrochloric acid and hydrofluoric acid, and the concentration of hydrochloric acid is
25wt% to 35wt%, the concentration of hydrofluoric acid is 40wt% to 50wt%, soaks tantalum ingot 5min in Acidwash solution under normal temperature and arrives
15min；
Step 8 is stocked up：Stocked up with 800mm milling trains to 0.5mm-0.8mm；
Step 9 vacuum annealing is heat-treated：Control vacuum 0.001Pa, 900 DEG C to 1300 DEG C of maximum temperature, in the highest temperature
Lower soaking time 90min to the 120min of degree；
Step 10 rolls：With 300mm band and strip rolling mills, it is 0.05mm High-purity Tantalum foils to produce thickness.
Further, as a further improvement on the present invention, it is characterised in that：The step 3 in metallic crystal process also
Additional electromagnetic field purifies, and controls magnetic field intensity 4800-600A/m.
Further, as a further improvement on the present invention, it is characterised in that：Electron beam furnace melting in the step 3
For zone refining, at a temperature of 2900 DEG C -3500 DEG C, the long and narrow material ingot shapes of local electronic Shu Jiare are into a narrow melting
Area, and electron beam is heated by mobile, this narrow melting zone is slowly moved along material ingot in certain direction, using impurity in solid phase
With liquid phase homostasis concentration difference, during being repeatedly melted and solidifying, impurity segregation is set to be able into solid phase or liquid phase
Remove or redistribute.
Further, as a further improvement on the present invention, it is characterised in that the melting zone uses resistance heating, and
By mobile adding thermal resistance, this narrow melting zone is set slowly to be moved along material ingot in certain direction, using impurity in solid phase and liquid phase
Homostasis concentration difference, during being repeatedly melted and solidifying, make impurity segregation be able to remove into solid phase or liquid phase or
Redistribution.
Further, as a further improvement on the present invention, it is characterised in that the melting zone uses sensing heating, and
By mobile heat induced, the narrow melting zone is set slowly to be moved along material ingot in certain direction, using impurity in solid phase and liquid
Identical equilibrium concentration difference, during being repeatedly melted and solidifying, impurity segregation is set to be removed into solid phase or liquid phase
Or redistribution.
Further, as a further improvement on the present invention, it is characterised in that：Secondary smelting repeats to walk in the step 5
Rapid 3 number is 1 time, 2 times or 3 times.
Further, as a further improvement on the present invention, it is characterised in that：In the step 6 during tandem rolling
Add intermediate annealing process.
Further, as a further improvement on the present invention, it is characterised in that：The first of tandem rolling in the step 6
Secondary rolling direction is vertical with second of rolling direction.
Further, as a further improvement on the present invention, it is characterised in that：The first of tandem rolling in the step 6
Secondary rolling direction is with second of rolling direction into 15 ° to 85 °.
By above technical scheme, the technique effect that the present invention realizes is：
1. tantalum foil impurity content is few, purity is high, specifically, is realized from the following aspects：
1) electronic torch melting is used：(2600-3000 DEG C) vacuum melting refers to remove Gases In Metals under vacuum
The process of impurity, actually reduce the solubility of gaseous impurity in a metal.According to Xi Weici laws, diatomic gas under constant temperature
The square root of body solubility in a metal and partial pressure is directly proportional.Therefore the vacuum of system is improved, just equivalent to reduction
The partial pressure of gas, the solubility of gas in a metal can be also reduced, and the portion gas impurity more than solubility will be from gold
Escape and remove in category.
Under the conditions of high vacuum (2.5-6 μ Pa), moisture drastically volatilizees at 100-200 DEG C, 600-700 DEG C of hydride decomposition
Effusion, alkali metal and its compound are volatilized at a temperature of 1100-1600 DEG C, and most of iron, nickel, chromium etc. are with low melting point oxide shape
State is volatilized, nitrogen volatilization effusion at 2300 DEG C, contrast hydrogen, the nitrogen oxygen big to metal affinity, then with add carbon deoxidation ([C]+[O]=
CO ↑) and above foreign metal low oxide MeON mode remove.
2) area smelting refinement is used：(2900-3150 DEG C) zone refining is a kind of method that depth is purified metals, in fact
Matter is into a narrow melting zone by the long and narrow material ingot shape of local heating, and mobile heating makes this narrow melting zone by certain side
Slowly moved to along material ingot, using impurity in solid phase and liquid phase homostasis concentration difference, during being repeatedly melted and solidifying,
Impurity just segregates in solid phase or liquid phase and is able to remove or redistributes；Melting zone typically uses resistance heating, sensing heating or
Electron beam heats.
3) purified using electromagnetic field：The depth purification high-melting-point gold under electromagnetic field (magnetic field intensity 4800-6000A/m) effect
The technology of category is used more and more.Electromagnetic field is not limited to the stirring action to molten metal, and more important is under electromagnetic field
Molten metal can be made to obtain being uniformly distributed for fault of construction, and refined grain structure in crystallization process.Crystallized in multiphase system
When, it can separate out the second phase orientation using electromagnetic field, electromagnetic field plays energy supporting role and stirring action, utilizes the evaporation of impurity
The second phase (oxide, carbide etc.), which is walked, with drift carrys out purified metal.
4) speed of melting, time are made according to how much selections of material, in fusion process by controlling precisely sweeping for electron beam
Retouch, control the purity of metal and the volatilization of impurity to remove with maximum efficiency.
In the case of from high-purity tantalum foil, ensure smelting temperature >=3050 DEG C, low-melting-point metal impurity content is respectively less than
1ppm, the impurity contents such as Nb, W are effectively reduced, so as to obtain high-purity nickel ingot.When melting vacuum is≤1 × 10-2pa
It can ensure that gaseous impurity content is very low, C, N, O are respectively less than 50ppm；Multiple smelting metal tantalum ingot purity can be higher.The present embodiment
Impurity analysis result is shown in《Impurity analysis result GDMS results》, as seen from the table, Nb, W content control are comparatively ideal in tantalum ingot
Value, other constituent contents also control more significant, so as to ensure that tantalum ingot purity >=99.99%.
2. tantalum foil fault of construction is few, grainiess is careful, the uniformity is high, sheet material interior mechanics performance isotropism
Height, specifically, realized from the following aspects：
1) rolling mill practice：High-performance OLED has high want with high-purity tantalum foil to metal purity, grain size and uniformity
Ask, this technique is since strict control into factory's raw material metal impurity content, in tantalum foil forms process, using large deformation
Tandem rolling and intermediate annealing process are measured, optimizes rolling technological parameter and annealing temperature, ensures the mechanical property of sheet material respectively to same
Property, uniform, tiny grain structure is obtained after annealing.
2) hammer cogging is not used, high-power milling train cogging is directly carried out, simplifies technological process, improves work effect
Rate.
By this project implementation, it can produce and meet the high-purity tantalum foils of OLED, its size can reach：0.05*280*
Lmm, purity reach 99.99%.
Impurity content standard (max.ppm)：
Claims (9)
- The high-purity tantalum foil preparation methods of 1.OLED, it is characterised in that comprise the following steps：Step 1 is stocked up：Select niobium, W content low, the tantalum bar of purity >=99.8%；Step 2 shove charge：Clearing furnace, ensure to clear up reactor without the debris that drops in vacuum chamber, avoid polluting, keep high-purity ring Border, tantalum bar tie up material shove charge；Step 3 melting once：Using electron beam furnace melting, melting is started to warm up in burner hearth vacuum≤0.006pa, remains molten Refine temperature >=3050 DEG C, according to melting tantalum bar quality how much, control smelting time, refining speed is maintained at≤45kg/h, and moderately The accurate distribution of electron beam is manipulated, ensures fully to melt tantalum bar；Step 4 vacuum cooled：The High-purity Tantalum ingot that melting is completed, 8h~12h is cooled down under vacuum conditions and is come out of the stove；Step 5 secondary smelting：Repeat step 3；Step 6 split rolling method：Using 2000 tons of 1.2 meters of reversible cold, hot two-purpose milling trains, using the method for tandem rolling, and control The drafts rolled each time is between 12% to 18%；Step 7 tantalum ingot pickling：Acidwash solution formula is arrived using hydrochloric acid and the mixed solution of hydrofluoric acid, the concentration of hydrochloric acid for 25wt% 35wt%, the concentration of hydrofluoric acid is 40wt% to 50wt%, and tantalum ingot 5min to 15min is soaked in Acidwash solution under normal temperature；Step 8 is stocked up：Stocked up with 800mm milling trains to 0.5mm-0.8mm；Step 9 vacuum annealing is heat-treated：Control vacuum 0.001Pa, 900 DEG C to 1300 DEG C of maximum temperature, at the maximum temperature Soaking time 90min to 120min；Step 10 rolls：With 300mm band and strip rolling mills, it is 0.05mm High-purity Tantalum foils to produce thickness.
- 2. the high-purity tantalum foil preparation methods of OLED according to claim 1, it is characterised in that：The step 3 is in metal knot Brilliant process also additional electromagnetic field purifies, and controls magnetic field intensity 4800-600A/m.
- 3. the high-purity tantalum foil preparation methods of OLED according to claim 1, it is characterised in that：Electronics in the step 3 The melting of beam stove is zone refining, and at a temperature of 2900 DEG C -3500 DEG C, the long and narrow material ingot shapes of local electronic Shu Jiare are narrow into one Melting zone, and heat electron beam by mobile, this narrow melting zone is slowly moved along material ingot in certain direction, utilize impurity In solid phase and liquid phase homostasis concentration difference, during being repeatedly melted and solidifying, make impurity segregation into solid phase or liquid phase And it is able to remove or redistributes.
- 4. the high-purity tantalum foil preparation methods of OLED according to claim 3, it is characterised in that the melting zone uses resistance Heating, and by mobile adding thermal resistance, this narrow melting zone is slowly moved along material ingot in certain direction, using impurity in solid phase With liquid phase homostasis concentration difference, during being repeatedly melted and solidifying, impurity segregation is set to be able into solid phase or liquid phase Remove or redistribute.
- 5. the high-purity tantalum foil preparation methods of OLED according to claim 3, it is characterised in that the melting zone use feeling should Heating, and by mobile heat induced, the narrow melting zone is slowly moved along material ingot in certain direction, using impurity solid Mutually with liquid phase homostasis concentration difference, during being repeatedly melted and solidifying, impurity segregation is set to be obtained into solid phase or liquid phase To remove or redistribute.
- 6. the high-purity tantalum foil preparation methods of OLED according to claim 1, it is characterised in that：It is secondary molten in the step 5 The number for refining repeat step 3 is 1 time, 2 times or 3 times.
- 7. the high-purity tantalum foil preparation methods of OLED according to claim 1, it is characterised in that：Intersect in the step 6 and roll Intermediate annealing process is added during system.
- 8. the high-purity tantalum foil preparation methods of OLED according to claim 1, it is characterised in that：Intersect in the step 6 and roll The first time rolling direction of system is vertical with second of rolling direction.
- 9. the high-purity tantalum foil preparation methods of OLED according to claim 1, it is characterised in that：Intersect in the step 6 and roll The first time rolling direction of system is with second of rolling direction into 15 ° to 85 °.
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| CN107858523A (en) * | 2017-12-27 | 2018-03-30 | 清远先导材料有限公司 | The purifying plant and method of a kind of high purity indium |
| CN107858523B (en) * | 2017-12-27 | 2019-11-12 | 清远先导材料有限公司 | A kind of purifying plant and method of high purity indium |
| CN109371255A (en) * | 2018-10-30 | 2019-02-22 | 金川集团股份有限公司 | A kind of 6N high-purity cobalt ingot casting method |
| CN109371255B (en) * | 2018-10-30 | 2020-05-05 | 金川集团股份有限公司 | 6N high-purity cobalt ingot casting method |
| CN111440938A (en) * | 2020-04-21 | 2020-07-24 | 合肥工业大学 | Annealing strengthening process method for rolling pure tantalum foil |
| CN111440938B (en) * | 2020-04-21 | 2022-01-28 | 合肥工业大学 | Annealing strengthening process method for rolling pure tantalum foil |
| CN111893311A (en) * | 2020-08-07 | 2020-11-06 | 上海大学 | Device and method for removing impurity elements in electron beam smelting process by using static magnetic field acceleration |
| CN114178788A (en) * | 2021-12-06 | 2022-03-15 | 天津大学 | Method for regulating impurity distribution and further improving metal surface processing quality based on surface layer region smelting |
| CN114433847A (en) * | 2022-02-11 | 2022-05-06 | 寰采星科技(宁波)有限公司 | Preparation method of high-cleanness metal foil and preparation method of metal mask strip |
| CN115572843A (en) * | 2022-10-26 | 2023-01-06 | 江苏美特林科特殊合金股份有限公司 | Preparation method of high-purity metal tantalum |
| CN115572843B (en) * | 2022-10-26 | 2023-08-29 | 江苏美特林科特殊合金股份有限公司 | Preparation method of high-purity metal tantalum |
| CN116812931A (en) * | 2023-06-13 | 2023-09-29 | 辽宁中色新材科技有限公司 | Environment-friendly production process of dititanium carbide MXene material |
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