CN105127232A - New high-temperature high specific strength niobium alloy wire processing process - Google Patents
New high-temperature high specific strength niobium alloy wire processing process Download PDFInfo
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- CN105127232A CN105127232A CN201510227825.1A CN201510227825A CN105127232A CN 105127232 A CN105127232 A CN 105127232A CN 201510227825 A CN201510227825 A CN 201510227825A CN 105127232 A CN105127232 A CN 105127232A
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Abstract
The present invention relates to a new high-temperature high specific strength niobium alloy wire processing process which is characterized by comprising the following steps: (1) sheared billet rotary swaging, to be more specific, a niobium alloy cast ingot is extruded or forged to prepare a sheared billet with the diameter of 30-60 mm, a wire billet with the diameter of 2.0-6.0 mm can be processed by multi-pass rotary swaging and heat treatment of the sheared billet; (2) surface oxidizing and film coating; (3) wire drawing, to be more specific, a finished wire with the diameter of 0.5-4.0 mm can be processed by multi-pass rotary drawing and two times of heat treatment of the wire billet with the diameter of 2.0-6.0 mm; (4) acid washing; and (5) finished product heat treatment. The new high-temperature high specific strength niobium alloy wire uses metal niobium as a substrate, and the wire obtained by the process significantly improves the high temperature mechanical properties of the metal niobium and has stable performance and even ingredients by solid solution strengthening and precipitation strengthening typical strengthening ways.
Description
Technical field
The present invention relates to a kind of processing technology of new type high temperature high-specific strength niobium alloy silk material.
Background technology
Along with the development of aeronautical and space technology, the performance requirement of aerospace material is improving constantly.In the multiple high-temperature alloy material such as tantalum, niobium, molybdenum, tungsten that various countries develop, niobium series alloy with its excellent mechanical behavior under high temperature, processability and low-density, low cost etc. in aerospace material always in occupation of critical role.
The U.S. is 1400 DEG C, 1500 DEG C in short-term in the trade mark C103 niobium alloy serviceability temperature that nineteen sixty-five develops, 42MPa is also had at 1500 DEG C of Tensile strength, any iron-based, nickel-base alloy cannot be equal to, this alloy is widely used in spacecraft heat resistant structure, comprises all kinds of satellite, airship radiation cools rail, appearance control thrust chamber chamber wall materials.But along with the development of space technology, more high performance requirements is proposed to engine, corresponding requirements material has more operation at high temperature, external one side finds the higher material of heatproof, as rhenium base (iridium coating layer) material succeeded in developing the eighties, operating temperature can up to 2200 DEG C, but this kind of material is heavier than niobium alloy a lot of and raw material is rare, processing technology is complicated.Another developing direction is the existing niobium alloy of improvement, improves its serviceability temperature, and the U.S. develops again as Nb-W-Mo-Zr series etc. can weld high-strength niobium alloy, and suitable when hot strength and C103 alloy 1500 DEG C when its 1750 DEG C, serviceability temperature can reach more than 1650 DEG C in short-term; The Soviet Union also mainly concentrates in this period and studies Nb-W-Mo-Zr series niobium alloy, and as the trade mark 5 в м ц niobium alloy, its 1700 DEG C is that hot strength reaches about 60MPa.
Summary of the invention
The object of this invention is to provide a kind of processing technology of new type high temperature high-specific strength niobium alloy silk material, the mechanical behavior under high temperature of metal niobium can be significantly improved, and stable performance, uniform ingredients, 1400 DEG C time, hot strength can reach 190MPa.
A processing technology for new type high temperature high-specific strength niobium alloy silk material, its special feature is, comprises the steps:
(1) excellent base is swaged: by niobium alloy ingot casting through extruding or the obtained diameter of forging processing
the excellent base of mm, swages and heat treatment through multi-pass, is machined to diameter
line base; Wherein every time working modulus of swaging controls between 10%-25%;
Wherein carry out a pickling degreasing after every time processing of swaging: configuration mixed acid, then the attachment on the line base that obtains is removed in pickling;
Wherein carry out an intermediate heat-treatment after every time processing of swaging: heat treatment temperature is 1400-1550 DEG C, and temperature retention time is 60-120min; And the general working rate between twice heat treatment controls between 50%-85%;
(2) surface oxidation overlay film: air atmosphere or have an oxygen atmosphere resistance furnace in overlay film, control coated temperature 400-600 DEG C, overlay film time 5-20min;
(3) silk material drawing: by the diameter obtained
line base, through multi pass drawing and twice heat treatment, obtains diameter
finished silk material; Wherein every time drawing working modulus controls between 10%-30%, and the general working rate between twice heat treatment controls between 50%-90%;
(4) pickling: configuration mixed acid, the attachment on the finished silk material that then pickling removal step (5) obtains;
(5) finished product heat treatment: heat treatment temperature is 1300 ~ 1450 DEG C, temperature retention time is 60 ~ 120min.
The mixed acid of step (1) and (4) middle configuration is according to volume ratio HNO
3: HF:H
2the mixed acid of O=10:1:5.
The new type high temperature high-specific strength niobium alloy (trade mark Nb521) adopted in present invention process is using metal niobium as matrix, add the refractory metal elements such as tungsten, molybdenum and zirconium, the silk material that this technique obtains significantly improves the mechanical behavior under high temperature of metal niobium by the typical schedule of reinforcement of solution strengthening and precipitation strength, and stable performance, uniform ingredients, 1400 DEG C time, hot strength reaches 190MPa, exceeds nearly 4 times than C103 alloy; 1600 DEG C time, hot strength reaches more than 70MPa, and 1800 DEG C time, hot strength still maintains more than 50MPa, and Aero-Space heat resistant structure material operating temperature is improved more than 200 DEG C by this novel niobium alloy.
Detailed description of the invention
Along with the development of space technology, current material cannot meet 1500 DEG C and more use under operation at high temperature condition.And present invention process is to new type high temperature high-specific strength niobium alloy, and (raw material components is Nb-5Mo-2Zr-1C, trade mark Nb521) excellent base through swaging, surface coating and drawing processing, be equipped with suitable Technology for Heating Processing and pickling degreasing technique, obtain swivel nut blank---the diameter being applied to rocket and the use of the high temperature particular surroundings such as the control of guided missile appearance and precise tracking material
silk material.Nb521 alloy bar base is obtained diameter by processing mode of swaging by present invention process
line base; Again through surface coating process and drawing, acquisition surface-brightening, the finished silk material that dimensional accuracy is high.
The major advantage of present invention process is: give full play to by adopting the three-dimensional compressive stress stress of processing mode of swaging that this strong hardness of Nb521 alloy is high, the low drawing abillity of plasticity; By suitable Technology for Heating Processing, reach elimination material internal stress, recover moulding, to realize continuing the object of processing; Surface coating is carried out to the line base after heat treatment, between online base matrix surface and drawing die nib, forms one deck barrier film, avoid occurring that silk material surface mucosa etc. affects drawing and processes the defect of carrying out; Processed by drawing, can obtain that dimensional accuracy is high, the finished silk material of surface-brightening.
Embodiment 1:
The procedure of processing of niobium alloy bar material of the present invention is:
1. rod base swages 1: the extruding of Nb521 niobium alloy or forging are obtained Φ 60mm niobium alloy rod base, processing of swaging is carried out after 1550 DEG C × 100min heat treatment, Φ 60mm → Φ 56mm (pass reduction ε=12.9%) → Φ 53mm (ε=12.9%) → Φ 53mm (ε=10.4%) → Φ 50mm (ε=11%) → Φ 47mm (ε=11.6%) → Φ 44mm (ε=12.3%) → Φ 41mm (ε=13.2%, ε
always=53.3%), feed rate of swaging 5 ~ 10mm/s, checks excellent base surface after every time processing of swaging, and carries out lower a time again and to swage processing, will carry out defect repair if desired after confirming unfolded and serious scratch.
2. pickling degreasing 1: according to volume ratio HNO
3(69.2%): HF (40%): H
2o=10:1:5 configures mixed acid and carries out pickling, and object removes surface impurity, visually observes visible metallic luster.Certainly also optional with having other concentration of same effect, the mixed acid of component proportion.
3. intermediate heat-treatment 1: heat treatment temperature is 1500 DEG C, temperature retention time is 100min.
4. rod base is swaged 2: Φ 41mm niobium alloy rod base → Φ 38mm (ε=14.1%) → Φ 35mm (ε=15.2%) → Φ 32mm (ε=16.4%) → Φ 30mm (ε=12.1%) → Φ 28mm (ε=12.9%) → Φ 26mm (ε=13.8%) → Φ 24mm (ε=14.8%) → Φ 22mm (ε=16.0%) → Φ 20mm (ε=17.4%, ε
always=76.2%), feed rate of swaging 10 ~ 20mm/s, checks excellent base surface after every time processing of swaging, and carries out lower a time again and to swage processing, will carry out defect repair if desired after confirming unfolded and serious scratch.
5. pickling degreasing 2: according to volume ratio HNO
3(69.2%): HF (40%): H
2o=10:1:5 configures mixed acid and carries out pickling, and object removes surface impurity, visually observes visible metallic luster.Certainly also optional with having other concentration of same effect, the mixed acid of component proportion.
6. intermediate heat-treatment 2: heat treatment temperature is 1450 DEG C, temperature retention time is 90min.
7. rod base is swaged 3: Φ 20mm niobium alloy rod base → Φ 18mm (ε=19.0%) → Φ 16mm (ε=21.0%) → Φ 14.5mm (ε=17.9%) → Φ 13mm (ε=19.6%) → Φ 11.5mm (ε=21.7%) → Φ 10mm (ε=24.4%, ε
always=75.0%), feed rate of swaging 10 ~ 20mm/s, checks excellent base surface after every time processing of swaging, and carries out lower a time again and to swage processing, will carry out defect repair if desired after confirming unfolded and serious scratch.
8. pickling degreasing 3: according to volume ratio HNO
3(69.2%): HF (40%): H
2o=10:1:5 configures mixed acid and carries out pickling, and object removes surface impurity, visually observes visible metallic luster.Certainly also optional with having other concentration of same effect, the mixed acid of component proportion.
9. intermediate heat-treatment 3: heat treatment temperature is 1450 DEG C, temperature retention time is 110min.
10. rod base is swaged 4: Φ 10mm niobium alloy rod base → Φ 9mm (ε=19.0%) → Φ 8mm (ε=21.0%) → Φ 7mm (ε=23.4%) → Φ 6.1mm (ε=24.1%) → Φ 15.3mm (ε=24.5%) → Φ 4.6mm (ε=24.7%) → Φ 4mm (ε=24.4%, ε
always=84.0%), feed rate of swaging 10 ~ 20mm/s, checks excellent base surface after every time processing of swaging, and carries out lower a time again and to swage processing, will carry out defect repair if desired after confirming unfolded and serious scratch.
11. pickling degreasing 4: according to volume ratio HNO
3(69.2%): HF (40%): H
2o=10:1:5 configures mixed acid and carries out pickling, and object removes surface impurity, visually observes visible metallic luster.Certainly also optional with having other concentration of same effect, the mixed acid of component proportion.
12. intermediate heat-treatment 4: heat treatment temperature is 1450 DEG C, temperature retention time is 80min.
13. surface oxidation overlay films: overlay film in air atmosphere or aerobic atmospheric resistance furnace, control coated temperature 500 DEG C, overlay film time 15min, overlay film color take navy blue as the best.
14. material drawings: Φ 4mm niobium alloy rod base → Φ 3.5mm (ε=23.4%) → Φ 3mm (ε=26.5%) → Φ 2.6mm (ε=24.9%) → Φ 2.2mm (ε=28.4%) → Φ 1.9mm (ε=25.4%) → Φ 1.65mm (ε=24.6%) → Φ 1.5mm (ε=17.4%, ε
always=86.0%), drawing speed 20 ~ 30mm/s, checks line base surface after every time drawing processing, confirms to carry out next passes of drawing processing again without after groove and serious scratch, will carry out defect repair if desired.
15. pickling: according to volume ratio HNO
3(69.2%): HF (40%): H
2o=10:1:5 configures mixed acid and carries out pickling, and object removes surface impurity, visually observes visible metallic luster.Certainly also optional with having other concentration of same effect, the mixed acid of component proportion.
16. finished product heat treatments: heat treatment temperature is 1350 DEG C, temperature retention time is 120min.
The niobium alloy of above-mentioned processes has high temperature high specific strength, and its high-temperature behavior is mainly determined by alloying component.Above-mentioned description of the process be the technique how obtaining this alloy wire, namely by adopting the three-dimensional compressive stress stress of processing mode of swaging to give full play to, this strong hardness of Nb521 alloy is high, the low drawing abillity of plasticity; By suitable Technology for Heating Processing, reach elimination material internal stress, recover moulding, to realize continuing the object of processing; Surface coating is carried out to the line base after heat treatment, between online base matrix surface and drawing die nib, forms one deck barrier film, avoid occurring that silk material surface mucosa etc. affects drawing and processes the defect of carrying out; Processed by drawing, can obtain that dimensional accuracy is high, the finished silk material of surface-brightening.
Claims (2)
1. a processing technology for new type high temperature high-specific strength niobium alloy silk material, is characterized in that, comprise the steps:
(1) excellent base is swaged: by niobium alloy ingot casting through extruding or the obtained diameter of forging processing
the excellent base of mm, swages and heat treatment through multi-pass, is machined to diameter
line base; Wherein every time working modulus of swaging controls between 10%-25%;
Wherein carry out a pickling degreasing after every time processing of swaging: configuration mixed acid, then the attachment on the line base that obtains is removed in pickling;
Wherein carry out an intermediate heat-treatment after every time processing of swaging: heat treatment temperature is 1400-1550 DEG C, and temperature retention time is 60-120min; And the general working rate between twice heat treatment controls between 50%-85%;
(2) surface oxidation overlay film: air atmosphere or have an oxygen atmosphere resistance furnace in overlay film, control coated temperature 400-600 DEG C, overlay film time 5-20min;
(3) silk material drawing: by the diameter obtained
line base, through multi pass drawing and twice heat treatment, obtains diameter
finished silk material; Wherein every time drawing working modulus controls between 10%-30%, and the general working rate between twice heat treatment controls between 50%-90%;
(4) pickling: configuration mixed acid, the attachment on the finished silk material that then pickling removal step (5) obtains;
(5) finished product heat treatment: heat treatment temperature is 1300 ~ 1450 DEG C, temperature retention time is 60 ~ 120min.
2. the processing technology of a kind of new type high temperature high-specific strength niobium alloy silk material as claimed in claim 1, is characterized in that: the mixed acid of step (1) and (4) middle configuration is according to volume ratio HNO
3: HF:H
2the mixed acid of O=10:1:5.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111715722A (en) * | 2020-06-19 | 2020-09-29 | 西安菲尔特金属过滤材料股份有限公司 | Preparation method of multi-core-number blended metal fiber for X and gamma ray protection |
| CN112453298A (en) * | 2020-11-03 | 2021-03-09 | 成都先进金属材料产业技术研究院有限公司 | Cold working method of high-temperature alloy rod and wire for fastener |
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| JPS60199522A (en) * | 1984-03-22 | 1985-10-09 | Natl Res Inst For Metals | Manufacture of superconductive alloy wire |
| CN101979171A (en) * | 2010-11-15 | 2011-02-23 | 宁夏东方钽业股份有限公司 | Processing technique for niobium alloy bar material |
| CN102011076A (en) * | 2010-11-15 | 2011-04-13 | 宁夏东方钽业股份有限公司 | Processing technique of niobium alloy plate |
| CN102921761A (en) * | 2012-11-08 | 2013-02-13 | 西安诺博尔稀贵金属材料有限公司 | Method for preparing niobium-zirconium alloy wire for electric light source |
| CN103611757A (en) * | 2013-12-10 | 2014-03-05 | 西部新锆核材料科技有限公司 | Method for preparing zirconium metal filaments |
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2015
- 2015-05-07 CN CN201510227825.1A patent/CN105127232A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60199522A (en) * | 1984-03-22 | 1985-10-09 | Natl Res Inst For Metals | Manufacture of superconductive alloy wire |
| CN101979171A (en) * | 2010-11-15 | 2011-02-23 | 宁夏东方钽业股份有限公司 | Processing technique for niobium alloy bar material |
| CN102011076A (en) * | 2010-11-15 | 2011-04-13 | 宁夏东方钽业股份有限公司 | Processing technique of niobium alloy plate |
| CN102921761A (en) * | 2012-11-08 | 2013-02-13 | 西安诺博尔稀贵金属材料有限公司 | Method for preparing niobium-zirconium alloy wire for electric light source |
| CN103611757A (en) * | 2013-12-10 | 2014-03-05 | 西部新锆核材料科技有限公司 | Method for preparing zirconium metal filaments |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111715722A (en) * | 2020-06-19 | 2020-09-29 | 西安菲尔特金属过滤材料股份有限公司 | Preparation method of multi-core-number blended metal fiber for X and gamma ray protection |
| CN111715722B (en) * | 2020-06-19 | 2022-05-27 | 西安菲尔特金属过滤材料股份有限公司 | Preparation method of multi-core-number blended metal fiber for X and gamma ray protection |
| CN112453298A (en) * | 2020-11-03 | 2021-03-09 | 成都先进金属材料产业技术研究院有限公司 | Cold working method of high-temperature alloy rod and wire for fastener |
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