CN101403097B - Method for high-temperature alloy vacuum diffusion connection with film as intermediate coat - Google Patents
Method for high-temperature alloy vacuum diffusion connection with film as intermediate coat Download PDFInfo
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- CN101403097B CN101403097B CN2008101724715A CN200810172471A CN101403097B CN 101403097 B CN101403097 B CN 101403097B CN 2008101724715 A CN2008101724715 A CN 2008101724715A CN 200810172471 A CN200810172471 A CN 200810172471A CN 101403097 B CN101403097 B CN 101403097B
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Abstract
The invention belongs to the technical field of high-temperature alloy bonding. To develop a novel high-temperature alloy bonding method and reduce diffused bonding temperature, the invention provides a novel vacuum diffused bonding method which carries out high temperature alloying by adopting a magnetron sputtering device to deposit a film on the surface of a piece to be connected as a bonding interlayer. The film prepared by magnetron sputtering has favorable bonding force with a substrate; the rete which is compact and uniform has the thickness between 0.05-10Mum, nanometer-level grain size and larger surface energy, thus being able to realize high-temperature alloy bonding on the condition of lower than the conventional diffused bonding temperature of 200-400 DEG C. Moreover, high-quality joints can be acquired by designing the constituents and the structure of the interlayer film. The bonding process can be realized in an ordinary vacuum diffusion furnace without shielding gas atmosphere, so the process is easy and practical.
Description
Technical field
The invention belongs to technical field of high-temperature alloy bonding, relating to a kind of is that the method that the diffusion of superalloy vacuum connects is carried out in the middle layer with the film.
Background technology
Superalloy has higher high temperature strength, good anti-oxidant and hot corrosion resistance, and over-all propertieies such as good fatigue property, fracture toughness property, plasticity are widely used in fields such as Aeronautics and Astronautics, nuclear industry, oil, chemical industry.Along with science and technology development, the accurate superalloy components that possesses high performance superalloy novel material and special service requirements continues to bring out, and this has proposed acid test to existing interconnection technique.For example at aviation field, the soldering of single crystal super alloy blade or TLP diffusion welding, because the influence that some elements infiltrate to the mother metal diffusion in welding temperature height, solder or the middle layer alloy, the problem that has nearly seam district recrystallize seriously reduces the performance of mother metal and the blade member safe reliability under arms the time.This has limited its design and application on aircraft and aircraft engine to a certain extent, develops new method of attachment and is necessary greatly.The solid film material is nano thin-film especially, and is on this specific direction of thickness, small-sized, it is the amount that microcosmic can be surveyed, and on thickness direction because the existence at surface, interface is interrupted the continuity of material, thus to rerum natura generation many and diverse influences.For example, because the influence of surface energy reduces or the like fusing point.The present invention's proposition as the middle layer, utilizes its bigger surface energy can realize connecting under lower temperature with film.By selection intermediate layer film, the design of thin membrane structure approaching the various factors that connection procedure influences joint and mother metal performance is control effectively simultaneously, thereby realize high-strength connection with being connected the mother metal composition.Magnetron sputtering is a kind of film preparation means commonly used, and film that makes and matrix have good bonding force, rete is evenly fine and close, and the film grain fineness number can reach nanometer scale.Therefore, the present invention adopts magnetron sputtering to prepare film carries out superalloy as the middle layer sky diffusion connection.
Summary of the invention
The object of the invention is to provide a kind of and realizes that under lower temperature a kind of of superalloy is that the method that the diffusion of superalloy vacuum connects is carried out in the middle layer with the film.
Technical scheme of the present invention is: comprise following processing step:
(1) treats web member and carry out surface treatment, polish step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph earlier, select whether carry out mechanical polishing as required again, be placed at last and carry out ultrasonic cleaning in the acetone soln;
(2) by magnetron sputtering equipment to be connected surface deposition film, film thickness is 0.05～10 μ m, grain fineness number is a nanometer scale;
(3) putting into the vacuum diffusion furnace, being not less than the temperature rise rate heating of 10 ℃/min, is that 750～950 ℃, pressure are the connection that constant voltage insulation 1～3h realizes superalloy under 10～30MPa in temperature.
Film to be connected surface deposition is the single or multiple lift structure.
The film of to be connected surface deposition is made through magnetron sputtering by pure metal target or alloys target.
When to be connected surface deposition film, adopt under heating or room temperature and carry out magnetron sputtering.
Advantage of the present invention is:
(1) adopt the present invention being lower than the connection that conventional diffusion connects realization superalloy under 200～400 ℃ of conditions of temperature.
(2) adopt the present invention by the composition of design intermediate layer film, the various factors that the structure control connection procedure influences joint and mother metal performance, realize high-strength connection.
(3) adopt the present invention in general vacuum diffusion furnace, can connect, need not protective atmosphere, simple for process.
Embodiment
(1) treats web member and carry out surface treatment, polish step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph earlier, select whether carry out mechanical polishing as required again, be placed at last and carry out ultrasonic cleaning in the acetone soln.
(2) pass through magnetron sputtering deposition pure metal or nickel-base alloy nano thin-film on to be connected surface, film thickness is 0.05～10 μ m; Sedimentary film is the single or multiple lift structure; In the sputter film-forming process, be chosen in as required and treat the web member surface under room temperature or the heated condition and carry out the magnetron sputtering film, to be connected Heating temperature is 200～600 ℃ when selecting heated condition.
(3) put into the vacuum diffusion furnace, vacuum tightness reaches 2.0 * 10 in stove
-3～4.0 * 10
-3Beginning temperature rise rate with 10 ℃/min during Pa and heat and regulate the pressure size simultaneously, is that 750～950 ℃, pressure are the connection that constant voltage insulation 1～3h realizes superalloy under 10～30MPa in temperature.
(4) after connection finished, the web member furnace cooling was cooled to 150 ℃ of unloadings, takes out when being cooled to room temperature.
Embodiment one
DD6 single crystal alloy surface to be connected is polished step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph, be placed on then and carry out ultrasonic cleaning in the acetone soln.At two DD6 single crystal alloy surface deposition nickel films to be connected, thickness is about 2.5 μ m to the pure nickel target of employing purity 〉=99.98% (weight) through JCK-500 type magnetic control platform.To be connected is put into the vacuum diffusion furnace and it is applied suitable pressure connecting, and vacuum tightness reaches 2.6 * 10 in stove
-3Beginning temperature rise rate with 10 ℃/min during Pa and heat and regulate the pressure size simultaneously, is that 870 ℃, pressure are that constant voltage insulation 2h spreads connection under the 20MPa in temperature.After connecting end, the web member furnace cooling is cooled to 150 ℃ of unloadings, takes out when being cooled to room temperature.With the tissue topography of scanning electron microscopic observation jointing as seen, middle layer nickel film and DD6 single crystal alloy mother metal matrix bond are good, and jointing dense non-porous hole has certain strength of joint.
Embodiment two
DZ22 directionally solidified superalloy, DS superalloy surface to be connected is polished step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph, be placed on then and carry out ultrasonic cleaning in the acetone soln.At two to be connected surface deposition films, thickness is about 3 μ m to employing Ni-20Cr alloys target through JCK-500 type magnetic control platform.Joint face is covered with to be connected of film and puts into the vacuum diffusion furnace and it is applied suitable pressure connecting, vacuum tightness reaches 2.8 * 10 in stove
-3Beginning temperature rise rate with 10 ℃/min during Pa and heat and regulate the pressure size simultaneously, is that 870 ℃, pressure are that constant voltage insulation 3h spreads connection under the 30MPa in temperature.After connecting end, the web member furnace cooling is cooled to 150 ℃ of unloadings, takes out when being cooled to room temperature.With the tissue topography of scanning electron microscopic observation jointing, can observe the master alloy layer film and DZ22 alloy mother metal matrix bond is good, jointing dense non-porous hole has certain strength of joint.
Embodiment three
DD6 single crystal alloy surface to be connected is polished step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph, be placed on then and carry out ultrasonic cleaning in the acetone soln.Adopt the pure nickel target of purity 〉=99.98% (weight), in JCK-500 type magnetic control platform to two DD6 single crystal alloy surface deposition nickel films to be connected.Treat web member before the deposit film and heat, Heating temperature is 300 ℃, begins deposit film after temperature is even, and thickness is about 2.5 μ m.Joint face is covered with to be connected of film and puts into the vacuum diffusion furnace and it is applied suitable pressure connecting, vacuum tightness reaches 2.5 * 10 in stove
-3Beginning temperature rise rate with 10 ℃/min during Pa and heat and regulate the pressure size simultaneously, is that 870 ℃, pressure are that constant voltage insulation 1h spreads connection under the 10MPa in temperature.After connecting end, the web member furnace cooling is cooled to 150 ℃ of unloadings, takes out when being cooled to room temperature.With the tissue topography of scanning electron microscopic observation jointing, can observe middle layer nickel film and DD6 single crystal alloy mother metal matrix bond is good, jointing dense non-porous hole has certain strength of joint.
Embodiment four
K403 alloy surface to be connected is polished step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph, be placed on then and carry out ultrasonic cleaning in the acetone soln.Adopt the pure nickel target and the Ni-20Cr alloys target of purity 〉=99.98% (weight), through JCK-500 type magnetic control platform at two to be connected surface deposition Ni-20Cr/Ni multilayer film.At first to be connected surface deposition pure nickel film, thickness is about about 0.5 μ m.Deposited film film then, thickness is about about 2 μ m.Deposit one deck pure nickel film at last again, thickness is about about 0.5 μ m.Deposition finishes to be connected is put into the vacuum diffusion furnace and it is applied suitable pressure connecting, and vacuum tightness reaches 3.2 * 10 in stove
-3Beginning temperature rise rate with 10 ℃/min during Pa and heat and regulate the pressure size simultaneously, is that 870 ℃, pressure are that constant voltage insulation 2h spreads connection under the 20MPa in temperature.With the tissue topography of scanning electron microscopic observation jointing, can observe film and K403 alloy mother metal matrix bond is good, jointing dense non-porous hole has certain strength of joint.
Claims (2)
1. one kind is that the method that the diffusion of superalloy vacuum connects is carried out in the middle layer with the film, it is characterized in that, comprises following processing step:
(1) treats web member and carry out surface treatment, polish step by step with 200#, 400#, 600#, 800#, 1000#, 2000# abrasive paper for metallograph earlier, select whether carry out mechanical polishing as required again, be placed at last and carry out ultrasonic cleaning in the acetone soln;
(2) by magnetron sputtering equipment to be connected surface deposition single layer structure film, film thickness is 0.05～10 μ m, grain fineness number is a nanometer scale;
(3) putting into the vacuum diffusion furnace, being not less than the temperature rise rate heating of 10 ℃/min, is that 750～950 ℃, pressure are the connection that constant voltage insulation 1～3h realizes superalloy under 10～30MPa in temperature.
2. according to claim 1 a kind of be that the method that superalloy vacuum diffusion connects is carried out in the middle layer with the film, it is characterized in that the film of to be connected surface deposition is made through magnetron sputtering by pure metal target or alloys target.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101724715A CN101403097B (en) | 2008-11-12 | 2008-11-12 | Method for high-temperature alloy vacuum diffusion connection with film as intermediate coat |
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| CN2008101724715A CN101403097B (en) | 2008-11-12 | 2008-11-12 | Method for high-temperature alloy vacuum diffusion connection with film as intermediate coat |
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| CN101403097B true CN101403097B (en) | 2010-10-27 |
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| CN105349964B (en) * | 2015-11-25 | 2018-05-22 | 中山德华芯片技术有限公司 | It prevents from depositing the method for having reactant and its by-product on MOCVD reaction chamber components |
| CN107297554B (en) * | 2016-04-15 | 2019-07-12 | 南京理工大学 | A method of high-volume fractional SiCp/Al composite material is connected based on nano-multilayer film self- propagating |
| CN105925948B (en) * | 2016-05-18 | 2019-05-14 | 哈尔滨工业大学（威海） | A kind of aluminum alloy surface activation connection method |
| CN107442922B (en) * | 2017-09-18 | 2020-10-09 | 上海航天精密机械研究所 | Method for diffusion bonding of dissimilar materials by using amorphous interlayer |
| CN114425647B (en) * | 2020-10-29 | 2023-08-18 | 哈尔滨工业大学（威海） | Method for connecting graphite film and copper |
| CN113695731B (en) * | 2021-09-02 | 2022-10-25 | 哈尔滨工业大学 | Method for performing metal/alloy low-temperature diffusion connection by utilizing electrodeposited nanocrystalline nickel intermediate layer |
| CN115821397A (en) * | 2022-12-22 | 2023-03-21 | 燕山大学 | Bonded copper single crystal and atomic-scale diffusion bonding process method thereof |
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