CN114769585B - Cold spray forming method of Cu-Cr-Nb alloy - Google Patents
Cold spray forming method of Cu-Cr-Nb alloy Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 24
- 238000009718 spray deposition Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 38
- 239000007921 spray Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 15
- 238000005507 spraying Methods 0.000 claims abstract description 14
- 238000010288 cold spraying Methods 0.000 claims abstract description 8
- 230000007547 defect Effects 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000012159 carrier gas Substances 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000003570 air Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 2
- 238000003754 machining Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005097 cold rolling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000005488 sandblasting Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000001856 aerosol method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000010290 vacuum plasma spraying Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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Abstract
本发明公开了一种Cu‑Cr‑Nb系合金的冷喷涂成形方法，包括：将筛选的Cu‑Cr‑Nb粉末材料烘干；将Cu‑Cr‑Nb粉末利用冷喷涂设备喷涂至基底材料上，获得Cu‑Cr‑Nb喷涂层；进行真空退火处理，以消除喷涂层的界面缺陷；精密加工去除基底材料，得到Cu‑Cr‑Nb系合金成形件。本发明的方法实现了Cu‑Cr‑Nb合金的快速成形，结合后续低温真空退火处理，进行组织优化，消除喷涂层内部的界面缺陷。由于采用了低温处理工艺，Cr2Nb相未发生粗化，保证了合金的力学性能，经冷喷涂成形的Cu‑Cr‑Nb合金的硬度可达200‑300HV，Cr2Nb相尺寸保持2‑8μm。
The invention discloses a cold spray forming method of Cu-Cr-Nb alloy, which includes: drying the screened Cu-Cr-Nb powder material; spraying the Cu-Cr-Nb powder onto the base material using cold spray equipment , obtain the Cu‑Cr‑Nb spray coating; perform vacuum annealing treatment to eliminate interface defects in the spray coating; remove the base material by precision machining to obtain Cu‑Cr‑Nb series alloy formed parts. The method of the present invention realizes the rapid forming of Cu-Cr-Nb alloy, and combines it with the subsequent low-temperature vacuum annealing treatment to optimize the structure and eliminate the interface defects inside the sprayed layer. Due to the low-temperature treatment process, the Cr 2 Nb phase does not coarsen, ensuring the mechanical properties of the alloy. The hardness of the Cu‑Cr‑Nb alloy formed by cold spraying can reach 200‑300HV, and the Cr2Nb phase size remains at 2‑8 μm.
Description
技术领域Technical field
本发明涉及铜合金制备技术领域，具体涉及一种Cu-Cr-Nb系合金的冷喷涂成形方法。The invention relates to the technical field of copper alloy preparation, and specifically relates to a cold spray forming method of Cu-Cr-Nb alloy.
背景技术Background technique
Cu-Cr-Nb合金中的强化相Cr2Nb相是一种金属间化合物，具有高熔点(约1730℃)与高温稳定性，使得该类合金具有优异的导电、热膨胀、抗蠕变、高强度、高延展性和优良抗低频疲劳等性能，是火箭发动机燃烧室内衬的理想材料。但是，由于合金在普通熔铸制备过程中的缓慢冷却会导致Cr2Nb相明显粗化，尺寸达到1厘米，失去强化效果。因此该类合金只能先通过气雾法制备粉末，以防止Cr2Nb相长大。为了将Cu-Cr-Nb材料应用于服役场景，还需要将Cu-Cr-Nb粉末固化成完全致密的块体材料。而目前采用的热等静压、真空等离子喷涂等技术采用的温度较高，仍会引起部分Cr2Nb相颗粒长大。此外，目前的热等静压、真空等离子喷涂等Cu-Cr-Nb粉末的固化工艺成本较高，效率较低，限制了该类材料的应用与推广。The strengthening phase Cr 2 Nb phase in Cu-Cr-Nb alloy is an intermetallic compound with a high melting point (about 1730°C) and high temperature stability, which makes this type of alloy have excellent electrical conductivity, thermal expansion, creep resistance, and high temperature resistance. With its strength, high ductility and excellent resistance to low-frequency fatigue, it is an ideal material for the lining of rocket engine combustion chambers. However, due to the slow cooling of the alloy during the ordinary melting and casting preparation process, the Cr 2 Nb phase will be significantly coarsened, reaching a size of 1 cm, and the strengthening effect will be lost. Therefore, this type of alloy can only be prepared into powder by aerosol method first to prevent the Cr 2 Nb phase from growing. In order to apply Cu-Cr-Nb materials to service scenarios, the Cu-Cr-Nb powder also needs to be solidified into a completely dense bulk material. However, the currently used technologies such as hot isostatic pressing and vacuum plasma spraying use relatively high temperatures, which will still cause some Cr 2 Nb phase particles to grow. In addition, the current solidification processes of Cu-Cr-Nb powder such as hot isostatic pressing and vacuum plasma spraying have high costs and low efficiency, which limits the application and promotion of this type of material.
专利CN111440963B、CN112553500A、CN110218897A中均采用气雾法制备Cu-Cr-Nb合金粉末，随后利用热压、SPS等工艺实现合金制备，粉末固化温度均高于800℃，在处理过程中无法避免Cr2Nb相发生粗化而降低合金性能。此外，以上方法的成本均较高，生产效率低。当前有关Cu-Cr-Nb合金制备方法，均存在一定的技术缺陷，难以有效抑制Cr2Nb相粗化并实现高效生产。Patents CN111440963B, CN112553500A, and CN110218897A all use the aerosol method to prepare Cu-Cr-Nb alloy powder, and then use hot pressing, SPS and other processes to achieve alloy preparation. The powder solidification temperatures are all higher than 800°C, and Cr 2 cannot be avoided during the processing. The Nb phase coarsens and reduces the alloy properties. In addition, the costs of the above methods are high and the production efficiency is low. The current preparation methods of Cu-Cr-Nb alloys all have certain technical flaws, making it difficult to effectively suppress the coarsening of the Cr 2 Nb phase and achieve efficient production.
发明内容Contents of the invention
针对上述已有技术存在的不足，本发明提供一种Cu-Cr-Nb系合金的冷喷涂成形方法。In view of the shortcomings of the above-mentioned prior art, the present invention provides a cold spray forming method of Cu-Cr-Nb alloy.
本发明是通过以下技术方案实现的。The present invention is achieved through the following technical solutions.
一种Cu-Cr-Nb系合金的冷喷涂成形方法，其特征在于，所述方法包括：A cold spray forming method of Cu-Cr-Nb alloy, characterized in that the method includes:
(1)将筛选的Cu-Cr-Nb粉末材料烘干；(1) Dry the screened Cu-Cr-Nb powder material;
(2)将经步骤(1)得到的Cu-Cr-Nb粉末利用冷喷涂设备喷涂至基底材料上，获得Cu-Cr-Nb喷涂层；(2) Spray the Cu-Cr-Nb powder obtained in step (1) onto the base material using cold spray equipment to obtain a Cu-Cr-Nb spray layer;
(3)对经步骤(2)得到的Cu-Cr-Nb喷涂层进行真空退火处理，以消除喷涂层的界面缺陷；(3) Perform vacuum annealing treatment on the Cu-Cr-Nb sprayed layer obtained in step (2) to eliminate interface defects in the sprayed layer;
(4)对经步骤(3)得到的喷涂层进行精密加工去除基底材料，得到Cu-Cr-Nb系合金成形件(板材或者圆筒形件)。(4) Precisely process the sprayed layer obtained in step (3) to remove the base material to obtain a Cu-Cr-Nb alloy formed part (plate or cylindrical part).
进一步地，所述步骤(1)中Cu-Cr-Nb粉末成分的原子百分比组成包括：Cr 4-8at.％，Nb2-4at.％，余量为Cu和不可避免的杂质。Further, the atomic percentage composition of the Cu-Cr-Nb powder component in step (1) includes: Cr 4-8at.%, Nb2-4at.%, and the balance is Cu and inevitable impurities.
进一步地，所述步骤(1)中Cu-Cr-Nb粉末粒径为20-50μm，粉末中Cr2Nb相尺寸小于8μm。Further, in step (1), the particle size of the Cu-Cr-Nb powder is 20-50 μm, and the Cr 2 Nb phase size in the powder is less than 8 μm.
进一步地，所述步骤(2)中基底材料为表面喷砂处理的铜板或圆筒形铜材。Further, in the step (2), the base material is a copper plate or cylindrical copper material with surface sandblasting treatment.
进一步地，所述步骤(2)中将基底材料固定在转速为80～150rpm的旋转轴上进行喷涂。Further, in step (2), the base material is fixed on a rotating shaft with a rotation speed of 80 to 150 rpm for spraying.
进一步地，所述步骤(2)中利用冷喷涂设备喷涂的工艺参数包括：载气为压缩空气、氮气或氩气中的一种，载气压力为2～6MPa，预热温度为400-500℃，基底材料表面与喷枪的喷嘴出口的距离为30～60mm，喷枪移动速度为3～10mm/s。Further, the process parameters for spraying with cold spray equipment in step (2) include: the carrier gas is one of compressed air, nitrogen or argon, the carrier gas pressure is 2-6MPa, and the preheating temperature is 400-500 ℃, the distance between the surface of the base material and the nozzle outlet of the spray gun is 30~60mm, and the moving speed of the spray gun is 3~10mm/s.
进一步地，所述步骤(3)中真空退火处理的退火温度为600℃～800℃，处理时间为1.5h～3h。Further, the annealing temperature of the vacuum annealing treatment in step (3) is 600°C to 800°C, and the treatment time is 1.5h to 3h.
进一步地，得到的Cu-Cr-Nb系合金成形件，显微组织中Cr2Nb相的尺寸为2-8μm，组织内部无界面缺陷，维氏硬度达到200～300HV。Furthermore, in the obtained Cu-Cr-Nb alloy formed part, the size of the Cr 2 Nb phase in the microstructure is 2-8 μm, there are no interface defects within the structure, and the Vickers hardness reaches 200-300HV.
本发明涉及的制备Cu-Cr-Nb系合金方法，是利用冷喷涂技术将固态金属粉末在低于材料熔点温度下利用高压气体将金属粉末加速至超音速并连续喷射至基底材料上，使粉末颗粒发生强烈塑性变形并堆积成块体的过程。是一种基于高变形速率、大变形的制造工艺。冷喷涂具有高沉积速率、涂层厚度不受限制、残余热应力较低、材料不易氧化等优点。The method for preparing Cu-Cr-Nb alloys involved in the present invention uses cold spray technology to accelerate solid metal powder to supersonic speed using high-pressure gas at a temperature lower than the melting point of the material and continuously sprays it onto the base material, so that the powder A process in which particles undergo strong plastic deformation and accumulate into blocks. It is a manufacturing process based on high deformation rate and large deformation. Cold spraying has the advantages of high deposition rate, unlimited coating thickness, low residual thermal stress, and the material is not easily oxidized.
本发明的有益技术效果，将冷喷涂技术应用于Cu-Cr-Nb粉末的固化成形，实现Cu-Cr-Nb合金的快速成形，结合后续低温真空退火处理，进行组织优化，消除喷涂层内部的界面缺陷。由于采用了低温处理工艺，Cr2Nb相未发生粗化，保证了合金的力学性能，经冷喷涂成形的Cu-Cr-Nb合金的硬度可达200-300HV，Cr2Nb相尺寸保持2-8μm。The beneficial technical effect of the present invention is that cold spray technology is applied to the solidification forming of Cu-Cr-Nb powder to realize rapid forming of Cu-Cr-Nb alloy, and combined with subsequent low-temperature vacuum annealing treatment, the structure is optimized and the internal problems of the sprayed layer are eliminated. Interface defects. Due to the low-temperature treatment process, the Cr 2 Nb phase does not coarsen, ensuring the mechanical properties of the alloy. The hardness of the Cu-Cr-Nb alloy formed by cold spraying can reach 200-300HV, and the Cr 2 Nb phase size remains 2- 8μm.
附图说明Description of drawings
图1为本发明得到的Cu-Cr-Nb合金显微组织形貌图。Figure 1 is a microstructure morphology diagram of the Cu-Cr-Nb alloy obtained by the present invention.
具体实施方式Detailed ways
下面结合附图和具体实施方式对本发明进行详细说明。The present invention will be described in detail below with reference to the drawings and specific embodiments.
除非另有定义，下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的，并不是旨在限制本发明的保护范围。除非另有特别说明，本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。Unless otherwise defined, all technical terms used below have the same meanings as commonly understood by those skilled in the art. The technical terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of the present invention. Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased in the market or prepared by existing methods.
实施例1：Example 1:
本实施例的Cu-Cr-Nb系合金冷喷涂制备方法，包括以下步骤：The cold spray preparation method of Cu-Cr-Nb alloy in this embodiment includes the following steps:
(1)选择原子百分比成分为Cu-4at.％Cr-2at.％Nb，粒径为25μm，Cr2Nb相尺寸小于5μm的粉末，在真空干燥箱中80℃条件下烘干30min得到冷喷涂粉末原料；选用冷轧后喷砂处理的电解铜板作为基底材料，基底材料固定在转速为120rpm的旋转轴上。(1) Select a powder with an atomic percentage composition of Cu-4at.% Cr-2at.% Nb, a particle size of 25 μm, and a Cr 2 Nb phase size less than 5 μm, and dry it in a vacuum drying oven at 80°C for 30 minutes to obtain cold spraying Powder raw material; electrolytic copper plate after cold rolling and sandblasting is selected as the base material, and the base material is fixed on the rotating shaft with a rotation speed of 120rpm.
步骤2、将Cu-Cr-Nb粉末利用冷喷涂设备喷涂至基底材料上，获得Cu-Cr-Nb喷涂层。冷喷涂的工艺参数为：载气为压缩空气，载气压力为3MPa，预热温度为420℃，基底材料表面与喷枪喷嘴出口的距离为50mm，喷枪以5mm/s移动速度上下移动。Step 2: Spray Cu-Cr-Nb powder onto the base material using cold spray equipment to obtain a Cu-Cr-Nb spray coating. The process parameters of cold spraying are: the carrier gas is compressed air, the carrier gas pressure is 3MPa, the preheating temperature is 420°C, the distance between the surface of the base material and the spray gun nozzle outlet is 50mm, and the spray gun moves up and down at a moving speed of 5mm/s.
步骤3、将步骤2获得的Cu-Cr-Nb喷涂层放入真空退火炉中进行650℃，保温2h的退火处理。Step 3. Place the Cu-Cr-Nb spray coating obtained in Step 2 into a vacuum annealing furnace for annealing at 650°C and holding for 2 hours.
步骤4、对步骤3退火处理的喷涂层进行车削加工去除基底材料，得到成品Cu-Cr-Nb合金成形件。合金中的Cr2Nb相尺寸仍保持小于5μm，合金硬度为215HV。Step 4: Carry out turning processing on the sprayed layer annealed in Step 3 to remove the base material to obtain the finished Cu-Cr-Nb alloy formed part. The size of the Cr 2 Nb phase in the alloy remains less than 5 μm, and the alloy hardness is 215HV.
实施例2：Example 2:
本实施例的Cu-Cr-Nb系合金冷喷涂制备方法，包括以下步骤：The cold spray preparation method of Cu-Cr-Nb alloy in this embodiment includes the following steps:
(1)选择原子百分比成分为Cu-8at.％Cr-4at.％Nb，粒径为50μm，Cr2Nb相尺寸2-5μm的粉末，在真空干燥箱中90℃条件下烘干20min得到冷喷涂粉末原料；选用冷轧后喷砂处理的电解铜圆筒作为基底材料，基底材料固定在转速为150rpm的旋转轴上。(1) Select a powder with an atomic percentage composition of Cu-8at.% Cr-4at.% Nb, a particle size of 50 μm, and a Cr 2 Nb phase size of 2-5 μm, and dry it in a vacuum drying oven at 90°C for 20 minutes to obtain cold Spray powder raw materials; use an electrolytic copper cylinder that is sandblasted after cold rolling as the base material, and the base material is fixed on a rotating shaft with a rotation speed of 150 rpm.
步骤2、将Cu-Cr-Nb粉末利用冷喷涂设备喷涂至基底材料上，获得Cu-Cr-Nb喷涂层。冷喷涂的工艺参数为：载气为氮气，载气压力为5MPa，预热温度为450℃，基底材料表面与喷枪喷嘴出口的距离为40mm，喷枪以6mm/s移动速度上下移动。Step 2: Spray Cu-Cr-Nb powder onto the base material using cold spray equipment to obtain a Cu-Cr-Nb spray coating. The process parameters of cold spraying are: the carrier gas is nitrogen, the carrier gas pressure is 5MPa, the preheating temperature is 450°C, the distance between the surface of the base material and the outlet of the spray gun nozzle is 40mm, and the spray gun moves up and down at a moving speed of 6mm/s.
步骤3、将步骤2获得的Cu-Cr-Nb喷涂层放入真空退火炉中进行700℃，保温3h的退火处理。Step 3. Place the Cu-Cr-Nb spray coating obtained in Step 2 into a vacuum annealing furnace for annealing at 700°C and holding for 3 hours.
步骤4、对步骤3退火处理的喷涂层进行车削加工去除基底材料，得到成品Cu-Cr-Nb合金圆筒形件。合金中的Cr2Nb相尺寸仍保持2-5μm，合金硬度为289HV。Step 4: Carry out turning processing on the sprayed layer annealed in Step 3 to remove the base material, and obtain the finished Cu-Cr-Nb alloy cylindrical part. The size of the Cr 2 Nb phase in the alloy remains 2-5μm, and the alloy hardness is 289HV.
实施例3：Example 3:
本实施例的Cu-Cr-Nb系合金冷喷涂制备方法，包括以下步骤：The cold spray preparation method of Cu-Cr-Nb alloy in this embodiment includes the following steps:
(1)选择原子百分比成分为Cu-6at.％Cr-3at.％Nb，粒径为40μm，Cr2Nb相尺寸为4-8μm的粉末，在真空干燥箱中85℃条件下烘干30min得到冷喷涂粉末原料；选用冷轧后喷砂处理的电解铜板作为基底材料，基底材料固定在转速为100rpm的旋转轴上。(1) Select a powder with an atomic percentage composition of Cu-6at.% Cr-3at.% Nb, a particle size of 40 μm, and a Cr 2 Nb phase size of 4-8 μm, and dry it in a vacuum drying oven at 85°C for 30 minutes to obtain Cold spray powder raw material; electrolytic copper plate treated with cold rolling and sandblasting is selected as the base material, and the base material is fixed on a rotating shaft with a rotation speed of 100rpm.
步骤2、将Cu-Cr-Nb粉末利用冷喷涂设备喷涂至基底材料上，获得Cu-Cr-Nb喷涂层。冷喷涂的工艺参数为：载气为氩气，载气压力为4MPa，预热温度为480℃，基底材料表面与喷枪喷嘴出口的距离为45mm，喷枪以4mm/s移动速度上下移动。Step 2: Spray Cu-Cr-Nb powder onto the base material using cold spray equipment to obtain a Cu-Cr-Nb spray coating. The process parameters of cold spraying are: the carrier gas is argon, the carrier gas pressure is 4MPa, the preheating temperature is 480°C, the distance between the surface of the base material and the spray gun nozzle outlet is 45mm, and the spray gun moves up and down at a moving speed of 4mm/s.
步骤3、将步骤2获得的Cu-Cr-Nb喷涂层放入真空退火炉中进行675℃，保温3h的退火处理。Step 3. Put the Cu-Cr-Nb spray coating obtained in step 2 into a vacuum annealing furnace for annealing at 675°C and holding for 3 hours.
步骤4、对步骤3退火处理的喷涂层进行车削加工去除基底材料，得到成品Cu-Cr-Nb合金板材。合金中的Cr2Nb相尺寸仍保持小于8μm，合金硬度为256HV。Step 4: Carry out turning processing on the sprayed layer annealed in Step 3 to remove the base material to obtain the finished Cu-Cr-Nb alloy plate. The size of the Cr 2 Nb phase in the alloy remains less than 8 μm, and the alloy hardness is 256HV.
以上所述的仅是本发明的较佳实施例，并不局限发明。应当指出对于本领域的普通技术人员来说，在本发明所提供的技术启示下，还可以做出其它等同改进，均可以实现本发明的目的，都应视为本发明的保护范围。What is described above is only the preferred embodiment of the present invention, and does not limit the invention. It should be pointed out that for those of ordinary skill in the art, under the technical inspiration provided by the present invention, other equivalent improvements can be made, all of which can achieve the purpose of the present invention, and should be regarded as the protection scope of the present invention.
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