CN104962764A - Functionalized treatment method of Ti-V-Al light memory alloy for structural connection of aerospace non-metal-matrix composites - Google Patents
Functionalized treatment method of Ti-V-Al light memory alloy for structural connection of aerospace non-metal-matrix composites Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 22
- 239000011156 metal matrix composite Substances 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 29
- 239000000956 alloy Substances 0.000 claims abstract description 29
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 12
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 238000005097 cold rolling Methods 0.000 claims abstract description 9
- 238000007306 functionalization reaction Methods 0.000 claims abstract 4
- 238000005098 hot rolling Methods 0.000 claims description 12
- 229910000734 martensite Inorganic materials 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- 238000005096 rolling process Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 230000007547 defect Effects 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012267 brine Substances 0.000 claims description 2
- 229910001651 emery Inorganic materials 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- 230000003446 memory effect Effects 0.000 abstract description 9
- 230000002441 reversible effect Effects 0.000 abstract description 9
- 229910010380 TiNi Inorganic materials 0.000 abstract description 8
- 230000000930 thermomechanical effect Effects 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
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- 238000005498 polishing Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 238000009864 tensile test Methods 0.000 description 1
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Abstract
本发明公开了一种航天非金属基复合材料结构连接用Ti-V-Al轻质记忆合金功能化处理方法，属于航天复合材料技术领域，本发明的方法是将电弧熔炼的Ti-V-Al合金铸锭固溶处理后进行热轧，到一定厚度后重新固溶处理并淬火，之后进行冷轧。对冷轧后的试样进行退火处理，即得到具有优异形状记忆效应的Ti-V-Al轻质记忆合金。本发明能大幅提高Ti-V-Al合金形状记忆效应，其完全可逆应变达到7.5％，是除TiNi合金外的最高值。经过热机械处理后的Ti-V-Al合金是一种在航空航天领域极具潜力的复合材料结构连接用轻质记忆合金。
The invention discloses a Ti-V-Al lightweight memory alloy functionalization treatment method for structural connection of aerospace non-metal matrix composite materials, which belongs to the technical field of aerospace composite materials. The method of the invention is to arc-smelt Ti-V-Al After the alloy ingot is solution treated, it is hot rolled, and after reaching a certain thickness, it is solution treated and quenched again, and then cold rolled. An annealing treatment is carried out on the sample after cold rolling to obtain a Ti-V-Al lightweight memory alloy with excellent shape memory effect. The invention can greatly improve the shape memory effect of Ti-V-Al alloy, and its complete reversible strain reaches 7.5%, which is the highest value except TiNi alloy. The Ti-V-Al alloy after thermomechanical treatment is a kind of lightweight memory alloy with great potential in the field of aerospace for composite material structure connection.
Description
技术领域technical field
本发明涉及航天复合材料技术领域，尤其涉及一种航天非金属基复合材料结构连接用Ti-V-Al轻质记忆合金功能化处理方法。The invention relates to the technical field of aerospace composite materials, in particular to a functionalized treatment method for Ti-V-Al lightweight memory alloy used for structural connection of aerospace non-metal matrix composite materials.
背景技术Background technique
航空航天工业发展中，设计师一直致力于飞行器质量的轻量化。现代非金属基复合材料具有高的比刚度和比强度，已成为现代飞行器首选结构材料之一。飞行器的结构减重可带来极其可观的收益。例如，对一枚小型洲际导弹弹头，减重1Kg，在有效载荷不变的情况下射程将增加15km。对于国际通信卫星V号而言，其中心承力筒铝合金改为复合材料结构，可减重9kg，仅此一项可使卫星增加2000条通信线路，运行期间可增加盈利3000万美元，相当于330万美元的收益。In the development of the aerospace industry, designers have been working on reducing the weight of aircraft. Modern non-metallic matrix composites have high specific stiffness and specific strength, and have become one of the preferred structural materials for modern aircraft. Structural weight reduction of aircraft can bring extremely considerable benefits. For example, for a small intercontinental missile warhead, if the weight is reduced by 1Kg, the range will increase by 15km when the payload remains the same. For Intelsat V, the aluminum alloy of its central load-bearing cylinder is changed to a composite material structure, which can reduce the weight by 9kg. This alone can add 2,000 communication lines to the satellite, and increase the profit by 30 million US dollars during the operation, which is equivalent to In proceeds of $3.3 million.
形状记忆合金是一类具有形状记忆效应和超弹性的结构功能一体化材料，在航空航天领域有着广泛的应用，其中最为成功的应用是作为连接件，包括管接头和紧固铆钉等。利用其形状记忆特性，可以实现非金属基复合材料的均载连接，避免冲击振动引起构件破坏。目前记忆合金连接件常用的是TiNi合金，其具有大完全可逆应变(约8％)。但是TiNi合金的密度较大(约6.9g/cm3)，大量应用将显著降低火箭的有效载荷。随着航天领域对结构减重的迫切需求，开发具有大完全可逆应变特性的新型复合材料连接用轻质记忆合金已成为相关领域研究热点。Shape memory alloy is a kind of structure-function integrated material with shape memory effect and superelasticity. It has a wide range of applications in the aerospace field, and the most successful application is as connectors, including pipe joints and fastening rivets. Utilizing its shape memory properties, the load-sharing connection of non-metal matrix composite materials can be realized, and the damage of components caused by impact vibration can be avoided. At present, TiNi alloy is commonly used for memory alloy connectors, which has a large and completely reversible strain (about 8%). However, the density of TiNi alloy is relatively high (about 6.9g/cm 3 ), and a large number of applications will significantly reduce the payload of the rocket. With the urgent need for structural weight reduction in the aerospace field, the development of new lightweight memory alloys for composite material connections with large and completely reversible strain characteristics has become a research hotspot in related fields.
Ti-V-Al合金是一种轻质记忆合金，其密度仅为4.5g/cm3，与纯钛相当，在航空航天领域具有广泛的应用前景。但是其形状记忆效应与TiNi合金相比还有较大差距，其完全可逆应变仅为3％，无法达到连接件的使用要求。Ti-V-Al alloy is a light-weight memory alloy with a density of only 4.5g/cm 3 , comparable to pure titanium, and has broad application prospects in the aerospace field. However, its shape memory effect is far behind that of TiNi alloys, and its fully reversible strain is only 3%, which cannot meet the requirements for connecting parts.
发明内容Contents of the invention
本发明的目的是为了解决Ti-V-Al合金的形状记忆效应较低的问题，提出了一种提高其形状记忆效应的热机械处理方法。The purpose of the present invention is to solve the problem of low shape memory effect of Ti-V-Al alloy, and propose a thermomechanical treatment method for improving its shape memory effect.
本发明采用如下技术方案：The present invention adopts following technical scheme:
本发明的提高复合材料结构连接用Ti-V-Al轻质记忆合金的功能化处理方法的具体步骤如下：The specific steps of the functionalized treatment method of Ti-V-Al lightweight memory alloy for improving composite material structure connection of the present invention are as follows:
(1)Ti-V-Al合金以高纯钛、V和Al为原料，采用非自耗电弧熔炼炉熔炼，在真空下以氩气保护状态下制备；(1) Ti-V-Al alloy is made of high-purity titanium, V and Al as raw materials, melted in a non-consumable arc melting furnace, and prepared under argon protection under vacuum;
(2)步骤(1)熔炼后的铸锭经机械抛光去除表面杂质，将铸锭在600℃-1200℃下真空保温2～24小时以实现合金成分均匀化，然后快速淬入冰盐水中，以形成热弹性马氏体；(2) Step (1) The ingot after smelting is mechanically polished to remove surface impurities, and the ingot is kept in vacuum at 600°C-1200°C for 2 to 24 hours to achieve uniform alloy composition, and then quickly quenched into iced brine, to form thermoelastic martensite;
(3)将热处理后的铸锭在800℃-900℃下保温20-40min后热轧，每次下轧量为10％，之后重新回炉保温5分钟，之后再继续热轧，当板材厚度为4mm时停止热轧；(3) Heat-treated ingots are kept at 800°C-900°C for 20-40min and then hot-rolled, each down-rolling amount is 10%, and then returned to the furnace for 5 minutes, and then continue hot-rolling. Stop hot rolling at 4mm;
(4)将热轧后的板材在800-1000℃下保温半小时后，快速淬入冰盐水中以获得马氏体，用砂轮将热轧造成的表面缺陷打磨干净；(4) After the hot-rolled plate is kept at 800-1000°C for half an hour, it is quickly quenched into ice-salt water to obtain martensite, and the surface defects caused by hot rolling are polished with a grinding wheel;
(5)将热轧后的板材进行冷轧，每次下轧量为2％，每道次轧制后用砂轮将冷轧造成的裂纹和表面缺陷打磨干净，冷轧至1.6mm时停止，总变形量为60％；(5) Carry out cold rolling to the plate after hot rolling, each down-rolling amount is 2%, after each pass rolling, the crack and surface defect caused by cold rolling are polished with emery wheel, stop when cold rolling reaches 1.6mm, The total deformation is 60%;
(6)将冷轧后的板材进行线切割后，封入真空度10-4～10-5Torr的石英管中，放入热处理炉中进行退火处理，退火温度为650℃-800℃，时间为0.5小时，获得处理后的马氏体。(6) After wire-cutting the cold-rolled plate, seal it in a quartz tube with a vacuum degree of 10 -4 to 10 -5 Torr, put it into a heat treatment furnace for annealing treatment, the annealing temperature is 650°C-800°C, and the time is After 0.5 hours, the treated martensite was obtained.
所述的Ti-V-Al轻质记忆合金为Ti-13V-3Al合金，其中Ti的原子个数比为84％，V的原子个数比为13％，Al的原子个数比为3％。The Ti-V-Al lightweight memory alloy is a Ti-13V-3Al alloy, wherein the atomic number ratio of Ti is 84%, the atomic number ratio of V is 13%, and the atomic number ratio of Al is 3%. .
步骤(1)中，原料高纯钛、V、和A的纯度为99.99wt.％。In step (1), the purity of the high-purity titanium, V, and A raw materials is 99.99wt.%.
步骤(1)中，真空熔炼的真空度为1×10-4Pa～1×10-5Pa。。In step (1), the vacuum degree of the vacuum smelting is 1×10 -4 Pa to 1×10 -5 Pa. .
步骤(1)中，熔炼过程中，为保证合金成分的均匀性，每个铸锭被反复翻转熔炼六次并加以磁力搅拌。In step (1), during the smelting process, in order to ensure the uniformity of the alloy composition, each ingot is repeatedly turned and smelted six times and magnetically stirred.
步骤(2)中，优选将铸锭在900℃下真空保温2小时以实现合金成分均匀化。In step (2), the ingot is preferably kept at 900° C. for 2 hours in vacuum to achieve homogenization of the alloy composition.
步骤(3)中，优选热处理后的铸锭在850℃下保温30min。In step (3), preferably, the heat-treated ingot is kept at 850° C. for 30 minutes.
步骤(4)中，优选热轧后的板材在900℃下保温。In step (4), preferably, the hot-rolled plate is kept at 900°C.
步骤(6)中，优选退火温度为700℃。In step (6), the preferred annealing temperature is 700°C.
本发明的积极效果如下：The positive effect of the present invention is as follows:
本发明通过一种新的热机械处理方法对非自耗电弧熔炼的Ti-V-Al合金进行处理，大幅提高其形状记忆效应，其完全可逆应变达到7.5％，是除TiNi合金外的最高值。此外，该合金密度为4.53g/cm3，低于密度为6.9g/cm3的TiNi合金。经过热机械处理后的Ti-V-Al合金是一种在航空航天领域极具潜力的复合材料结构连接用轻质记忆合金。The invention treats the non-consumable arc smelted Ti-V-Al alloy through a new thermomechanical treatment method, which greatly improves its shape memory effect, and its fully reversible strain reaches 7.5%, which is the highest except TiNi alloy. value. In addition, the alloy has a density of 4.53 g/cm 3 , which is lower than that of the TiNi alloy with a density of 6.9 g/cm 3 . The Ti-V-Al alloy after thermomechanical treatment is a kind of lightweight memory alloy with great potential in the field of aerospace for composite material structure connection.
附图说明Description of drawings
图1为变形量为6％时不同退火温度Ti-13V-3Al合金的室温加载-卸载曲线；Fig. 1 is the room temperature loading-unloading curve of Ti-13V-3Al alloy with different annealing temperatures when the deformation is 6%;
图中，1-退火温度650℃、2-退火温度900℃、3-退火温度700℃、4-退火温度750℃、5-退火温度800℃。In the figure, 1-annealing temperature 650°C, 2-annealing temperature 900°C, 3-annealing temperature 700°C, 4-annealing temperature 750°C, 5-annealing temperature 800°C.
图2为变形量为7.5％时700℃退火0.5小时Ti-13V-3Al合金的室温加载-卸载曲线。Fig. 2 is the room temperature loading-unloading curve of the Ti-13V-3Al alloy annealed at 700°C for 0.5 hour when the deformation amount is 7.5%.
由图2可以看出，本发明的方法处理后的马氏体在7.5％变形后变形可以完全恢复，没有残余应变。It can be seen from Fig. 2 that the martensite processed by the method of the present invention can recover completely after 7.5% deformation without residual strain.
具体实施方式Detailed ways
下面的实施例是对本发明的进一步详细描述。The following examples are further detailed descriptions of the present invention.
具体实施方式一：Specific implementation mode one:
本实施方式中Ti-V-Al合金由Ti，V和Al三种元素构成，其中Ti的原子个数比为84％，V的原子个数比为13％，Al的原子个数比为3％。In this embodiment, the Ti-V-Al alloy is composed of three elements: Ti, V and Al, wherein the atomic number ratio of Ti is 84%, the atomic number ratio of V is 13%, and the atomic number ratio of Al is 3. %.
本实施方式中Ti-13V-3Al合金是采用纯度为99.95wt.％的海绵钛、99.99wt.％的V、99.99wt.％的Al为原料，采用非自耗电弧熔炼炉熔炼，在真空抽至5×10-3Pa后制备。为保证合金成分的均匀性，每个铸锭被反复翻转熔炼六次并加以磁力搅拌。In this embodiment, the Ti-13V-3Al alloy is made of sponge titanium with a purity of 99.95wt.%, 99.99wt.% V, and 99.99wt.% Al as raw materials, and is melted in a non-consumable arc melting furnace. Prepared after pumping to 5×10 -3 Pa. In order to ensure the uniformity of the alloy composition, each ingot was turned and smelted six times and magnetically stirred.
熔炼后的铸锭经机械抛光去除表面杂质后重量约为60g。将铸锭在900℃下真空保温2小时以实现合金成分均匀化，然后淬入水中，以形成热弹性马氏体。The smelted ingot weighs about 60g after mechanical polishing to remove surface impurities. The ingot was held at 900°C for 2 hours under vacuum to homogenize the alloy composition, and then quenched into water to form thermoelastic martensite.
将热处理后的铸锭在850℃下保温半小时后热轧，每次下轧量为10％，之后重新回炉保温五分钟，之后再继续热轧。当板材厚度为4mm时停止热轧。The heat-treated ingot is kept at 850° C. for half an hour and then hot-rolled, each down-rolling amount is 10%, and then returned to the furnace for five minutes to keep warm, and then continue hot-rolling. Stop hot rolling when the plate thickness is 4mm.
将热轧后的板材在900℃下保温半小时后淬入水中以获得马氏体。用砂轮将热轧造成的表面缺陷打磨干净。The hot-rolled plate is kept at 900°C for half an hour and then quenched into water to obtain martensite. Use a grinding wheel to clean the surface defects caused by hot rolling.
将热轧后的板材进行冷轧，每次下轧量为2％。每道次轧制后用砂轮将冷轧造成的裂纹和表面缺陷打磨干净。冷轧至1.6mm时停止，总变形量为60％。The hot-rolled plate is cold-rolled, and the amount of down-rolling is 2%. After each pass of rolling, the cracks and surface defects caused by cold rolling are cleaned with a grinding wheel. The cold rolling stops at 1.6 mm, and the total deformation is 60%.
将冷轧后的板材进行线切割后，封入抽真空的石英管中，放入热处理炉中进行退火处理，退火温度分别为650℃，700℃，750℃，800℃，时间为0.5小时。另取一组样品进行固溶处理，固溶温度为900℃，时间为1小时。之后将石英管淬入水中并打碎，以获得马氏体。After wire-cutting the cold-rolled plates, they were sealed in a evacuated quartz tube and placed in a heat treatment furnace for annealing treatment. The annealing temperatures were 650°C, 700°C, 750°C, and 800°C for 0.5 hours. Another group of samples was taken for solution treatment at a solution temperature of 900°C for 1 hour. The quartz tube is then quenched in water and broken to obtain martensite.
将退火处理(固溶处理)后的拉伸试样标记一定长度l0后在室温下进行拉伸，拉伸速率为1％/分钟，不同热处理工艺的试样均应变至6％后卸载。将卸载后的试样加热至马氏体逆转变结束温度Af之上保温一分钟，使其形状回复，之后测量回复后的标记长度l1，由公式：The annealed (solution treated) tensile sample was marked with a certain length l0 and then stretched at room temperature with a tensile rate of 1%/min. The samples of different heat treatment processes were all strained to 6% and then unloaded. Heat the unloaded sample above the martensite reverse transformation end temperature A f and keep it warm for one minute to restore its shape, then measure the restored mark length l 1 , according to the formula:
[1-(l1-l0)/0.06l0]×6％[1-(l 1 -l 0 )/0.06l 0 ]×6%
计算其可恢复应变。Calculate its recoverable strain.
由上述实验得出700℃退火0.5小时可以得到最佳的形状记忆效应。From the above experiments, it can be concluded that annealing at 700°C for 0.5 hours can obtain the best shape memory effect.
将700℃退火0.5小时后的Ti-13V-3Al合金进行不同拉伸变形量的加载-卸载实验，并按上述方法测定其可逆应变。结果显示，合金的最大可逆应变为7.5％。超过此变形量，合金将发生不可逆变形，无法完全形状回复。The Ti-13V-3Al alloy annealed at 700°C for 0.5 hours was subjected to loading-unloading experiments with different tensile deformations, and its reversible strain was measured according to the above method. The results show that the maximum reversible strain of the alloy is 7.5%. Beyond this amount of deformation, the alloy will undergo irreversible deformation and will not recover its full shape.
本实施方式的有益效果是：本发明通过一种新的热机械处理方法对非自耗电弧熔炼的Ti-V-Al合金进行处理，大幅提高其形状记忆效应，其完全可逆应变达到7.5％，是除TiNi合金外的最高值。此外，该合金密度为4.53g/cm3，低于密度为6.9g/cm3的TiNi合金。经过热机械处理后的Ti-V-Al合金是一种在航空航天领域极具潜力的复合材料结构连接用轻质记忆合金。The beneficial effect of this embodiment is: the present invention treats the non-consumable arc smelted Ti-V-Al alloy through a new thermomechanical treatment method, greatly improving its shape memory effect, and its fully reversible strain reaches 7.5% , is the highest value except TiNi alloy. In addition, the alloy has a density of 4.53 g/cm 3 , which is lower than that of the TiNi alloy with a density of 6.9 g/cm 3 . The Ti-V-Al alloy after thermomechanical treatment is a kind of lightweight memory alloy with great potential in the field of aerospace for composite material structure connection.
具体实施方案二：Specific implementation plan two:
本实施方式与具体实施方案一不同的是：室温拉伸试验的拉伸速率为3％/min。The difference between this embodiment and the first embodiment is that the tensile rate of the tensile test at room temperature is 3%/min.
具体实施方案三：Specific implementation plan three:
本实施方案与具体实施方案一和二不同的是：固溶处理温度为850℃。The difference between this embodiment and specific embodiments 1 and 2 is that the solution treatment temperature is 850°C.
具体实施方案四：Specific implementation plan four:
本实施方案与具体实施方案一至三不同的是：合金熔炼后线切割成四块，酸洗去除氧化皮后重新熔炼三到四遍。The difference between this embodiment and specific embodiments 1 to 3 is that: after the alloy is smelted, it is wire-cut into four pieces, and after pickling to remove scale, it is re-smelted three to four times.
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although the embodiments of the present invention have been shown and described, those skilled in the art can understand that various changes, modifications and substitutions can be made to these embodiments without departing from the principle and spirit of the present invention. and modifications, the scope of the invention is defined by the appended claims and their equivalents.
Claims (9)
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| CN105316526A (en) * | 2015-12-07 | 2016-02-10 | 哈尔滨工业大学 | High temperature shape memory alloy with good memory effect and machining performance and preparation method thereof |
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| CN113559333A (en) * | 2021-06-07 | 2021-10-29 | 中国科学院金属研究所 | A medical nickel-titanium alloy with high anticoagulant function without surface treatment |
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| CN117107177B (en) * | 2023-08-30 | 2024-04-23 | 烟台大学 | Mechanical training method and device for realizing high strength and high hardness of Ti-V-Al-Zr memory alloy |
| CN118726881A (en) * | 2024-06-21 | 2024-10-01 | 烟台大学 | Laser shock processing method for gradient heterostructure of TiVAl memory alloy |
| CN118726881B (en) * | 2024-06-21 | 2024-12-24 | 烟台大学 | Laser impact treatment method for TiVAl memory alloy gradient heterostructure |
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