CN102873938B - Fe-Si-B amorphous alloy-copper laminated composite material and preparation method thereof - Google Patents
Fe-Si-B amorphous alloy-copper laminated composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Fe-Si-B amorphous alloy-copper laminated composite material and a preparation method thereof. A vacuum diffusion connection testing machine is used, and Fe-Si-B amorphous alloy and copper are welded to form the laminated composite material through a diffusion welding method. In preparation, at super-cooled liquid-phase region temperature of the amorphous alloy, plastic deformation is performed on the amorphous alloy and the copper through pressure effect, connection surface oxidation films are removed, fresh surfaces of the amorphous alloy and the copper are contacted tightly, connection interface diffusion process is promoted through thermal insulation and pressure maintaining simultaneously, and an iron-based amorphous-copper laminated composite material of a large size is prepared under the precondition that crystallization of the amorphous alloy is avoided. By adopting the technical scheme, process parameters are controlled strictly and accurately, and the large-size composite material with good connection performance and broadband shielding performance is obtained.
Description
Technical field
The present invention relates to field of composite material preparation, specifically a kind of preparation method of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.
Background technology
Glassy metal has the performance more excellent than conventional amorphous metal, as high strength, high tenacity, good wear resistance and corrosion resistance, excellent magnetic performance etc.Since the sixties in 19th century, professor Duwez of California Institute of Technology prepares amorphous state Au-Si alloy till now first, and glassy metal is the hot fields of various countries scientist research always.Some developed countries such as the U.S., Japan, drop into the application of substantial contribution development non-crystaline amorphous metal in national defence, Aero-Space, the solar wind collector that the such as U.S. makes of Zr base amorphous, successful collection high energy solar wind ion, and armor-piercing bullet armor-penetrating ability prepared by non-crystaline amorphous metal is also apparently higher than traditional tungsten alloy bullet.Iron-based amorphous alloy ribbon material is the important non-crystalline material that industrialization is produced, critical role is occupied in energy-economic transformer is promoted, Development of New Generation amorphous band high-speed continuous casting technique, amorphous composite material technology of preparing, and amorphous alloy transformer manufacturing process etc. has been put into China " 12 " new material major products catalogue.
Non-crystaline amorphous metal has application prospect widely at Aeronautics and Astronautics, military affairs and civil area, but due to non-crystaline amorphous metal size restriction and lower temperature-room type plasticity hinder the extensive use of non-crystaline amorphous metal as engineering material.And by means of traditional metal materials Physical and mechanical properties and ripe processing technology of preparing, prepare amorphous-conventional metals composite, for the application of popularization non-crystaline amorphous metal, there is huge facilitation.The preparation of amorphous-conventional metals composite can reduce the preparation cost of non-crystaline amorphous metal product, increases the dependability of non-crystaline amorphous metal, make simultaneously non-crystaline amorphous metal excellent properties be effectively played.
Fe-Si-B non-crystaline amorphous metal is one of amorphous alloy component of current minority commercialization, is widely used in the fields such as transformer at present.Because the amorphous formation ability of Fe-Si-B non-crystaline amorphous metal is low, single roller need be adopted the method preparation of band is got rid of when preparing Fe-Si-B non-crystaline amorphous metal, the method that this single roller gets rid of band only can prepare amorphous thin ribbon, and can not prepare the large scale non-crystaline amorphous metal being applicable to structure-function integration.
Summary of the invention
For overcoming the deficiency can not preparing the large scale non-crystaline amorphous metal being applicable to structure-function integration existed in prior art, the present invention proposes a kind of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material and preparation method thereof.
Fe-Si-B non-crystaline amorphous metal-copper laminar composite material of the present invention is made up of one deck Fe-Si-B amorphous thin ribbon and two-layer copper, and described Fe-Si-B amorphous thin ribbon is clipped between described two-layer copper.
Fe-Si-B amorphous thin ribbon of the present invention is GB 1K101; The copper adopted is fine copper rod or brass bar.
Preparation process of the present invention comprises the following steps:
Step 1, surface treatment; By the connecting surface sanding and polishing of Fe-Si-B amorphous and copper, and after removing copper surface oxide with 5% watery hydrochloric acid, in ethanol with Ultrasonic Cleaning 1min respectively in acetone, obtain the good Fe-Si-B amorphous of surface treatment and copper;
Step 2, precompressed; Fe-Si-B amorphous good for surface treatment is placed between two pieces of copper rods, defines the sample of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material; Described sample is put into diffusion in vacuum jockey, and carries out precompressed by diffusion in vacuum jockey to sample pressurization, described moulding pressure is 5MPa;
Step 3, diffusion connects; The process that described diffusion connects is: after vacuumizing diffusion in vacuum jockey, is warming up to 480 ~ 500 DEG C and is incubated with the heating rate of 10 ~ 30 DEG C/min to the sample being arranged in diffusion in vacuum jockey; When the temperature of sample rises to 480 ~ 500 DEG C, to described sample pressurization 70 ~ 90MPa and pressurize; Insulation and dwell time are 20 ~ 40min; After insulation and pressurize terminate, to sample release, sample cools to room temperature with the furnace simultaneously, takes out sample, obtains Fe-Si-B amorphous-copper laminar composite material.
What the present invention proposed forms Fe-Si-B amorphous-copper laminar composite material by Fe-Si-B amorphous thin ribbon and copper, and adopting the method for Diffusion Welding to prepare the method for Fe-Si-B amorphous-copper laminar composite material, the diffusion efficiently solved between non-crystaline amorphous metal with copper heterogenous metal is connected formation problems.Described diffusion welding method can obtain the linkage interface being better than original material property, extensive in aerospace field application prospect.The superplastic forming technology of Diffusion bonding techniques and non-crystaline amorphous metal combines, for realizing the connection of non-crystaline amorphous metal and conventional metals and shaping there is unique advantage, diffusion technology for welding more easily breaks through the size and dimension restriction of linkage interface simultaneously, widens the range of application of non-crystaline amorphous metal.
Due to the technique scheme that the present invention takes, the present invention is made to have following characteristics:
1) adopt vacuum atmosphere in preparation, be conducive to avoiding the oxide-film of the densification that material surface generates in connection procedure to the inhibition of Elements Diffusion, obtain the material that switching performance is good.
2) take full advantage of diffusion in vacuum joint test machine heating rate fast, temperature control, the feature that pressure stability error is little, strict accurate Controlling Technology parameter, has good directive significance to industrial production.
3) Fe-Si-B non-crystaline amorphous metal has excellent low-frequency magnetic shielding properties, and Cu has good radioshielding effect, and the diffusion being realized the two by the present invention is connected, and can prepare a kind of composite with wideband shielding properties.
4) this experiment adopts diffusion connecting process, in the supercooling liquid phase region temperature of non-crystaline amorphous metal, make non-crystaline amorphous metal and copper plastic deformation occur by pressure effect simultaneously, remove connecting surface oxide-film, make both unsalted surface close contacts, promoted the carrying out of linkage interface diffusion process by heat-insulation pressure keeping simultaneously, prepare under the prerequisite avoiding amorphous alloy crystallization large-sized Fe-based amorphous-copper laminar composite material.
Accompanying drawing 3 and the Fe-Si-B amorphous showed in accompanying drawing 4-copper laminar composite material sample interface connection state SEM pattern and TEM pattern prove that Fe-Si-B amorphous-copper laminar composite material prepared by the present invention achieves good diffusion and is connected, and achieve the metallurgical binding of atomic level between Fe-Si-B amorphous-copper.
Accompanying drawing explanation
Fig. 1 Fe-Si-B amorphous-copper laminar composite material preparation technology flow chart.
XRD collection of illustrative plates Fe-based amorphous under Fig. 2 Fe-Si-B amorphous-copper laminar composite material preparation technology.
Fig. 3 Fe-Si-B amorphous-copper laminar composite material sample interface connection state SEM pattern picture.
Fig. 4 Fe-Si-B amorphous-copper laminar composite material linkage interface TEM pattern picture.In figure:
1. non-crystaline amorphous metal 2. bronze medal
Detailed description of the invention
Embodiment one
The present embodiment is a kind of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.Described Fe-Si-B non-crystaline amorphous metal-copper laminar composite material is made up of one deck Fe-Si-B amorphous thin ribbon and two-layer copper, and described Fe-Si-B amorphous thin ribbon is clipped between described two-layer copper.
The Fe-Si-B amorphous thin ribbon that the present embodiment adopts is GB 1K101; The copper adopted is T2 fine copper rod.
The present embodiment also proposed a kind of method preparing Fe-Si-B non-crystaline amorphous metal-copper laminar composite material, comprises the following steps:
Step 1, surface treatment; By the surface finish polishing to be connected of Fe-Si-B amorphous and copper, and after removing copper surface oxide with 5% watery hydrochloric acid, in ethanol with Ultrasonic Cleaning 1min respectively in acetone.
Step 2, precompressed.The Fe-Si-B amorphous handled well is placed between two pieces of copper rods, defines the sample of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.Described sample is put into diffusion in vacuum jockey, and carries out precompressed by diffusion in vacuum jockey to sample pressurization, described moulding pressure is 5MPa.
Step 3, diffusion connects.Described diffusion connection is realized by diffusion in vacuum jockey, and detailed process is:
0.6 × 10 is evacuated to diffusion in vacuum jockey
-2after Pa, with the heating rate of 10 DEG C/min 480 DEG C be warming up to the sample being arranged in diffusion in vacuum jockey and be incubated.When the temperature of sample rises to 480 DEG C, to described sample pressurization 90MPa and pressurize; Insulation and dwell time are 40min.After insulation and pressurize terminate, unload be depressed into 2MPa to sample, sample cools to room temperature with the furnace simultaneously, takes out sample, obtains Fe-Si-B amorphous-copper laminar composite material.
Fe-Si-B amorphous through preparing the present embodiment-copper laminar composite material linkage interface is observed, and sample connects good, linkage interface is straight zero defect.
Embodiment two
The present embodiment is a kind of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.Described Fe-Si-B non-crystaline amorphous metal-copper laminar composite material is made up of one deck Fe-Si-B amorphous thin ribbon and two-layer copper, and described Fe-Si-B amorphous thin ribbon is clipped between described two-layer copper.
The Fe-Si-B amorphous thin ribbon that the present embodiment adopts is GB 1K101; The copper adopted is T2 fine copper rod.
The present embodiment also proposed a kind of method preparing Fe-Si-B non-crystaline amorphous metal-copper laminar composite material, comprises the following steps:
Step 1, surface treatment; By the surface finish polishing to be connected of Fe-Si-B amorphous and copper, and after removing copper surface oxide with 5% watery hydrochloric acid, in ethanol with Ultrasonic Cleaning 1min respectively in acetone.
Step 2, precompressed.The Fe-Si-B amorphous handled well is placed between two pieces of copper rods, defines the sample of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.Described sample is put into diffusion in vacuum jockey, and carries out precompressed by diffusion in vacuum jockey to sample pressurization, described moulding pressure is 5MPa.
Step 3, diffusion connects.Described diffusion connection is realized by diffusion in vacuum jockey, and detailed process is:
0.6 × 10 is evacuated to diffusion in vacuum jockey
-2after Pa, with the heating rate of 20 DEG C/min 490 DEG C be warming up to the sample being arranged in diffusion in vacuum jockey and be incubated.When the temperature of sample rises to 490 DEG C, to described sample pressurization 80MPa and pressurize; Insulation and dwell time are 30min.After insulation and pressurize terminate, unload be depressed into 2MPa to sample, sample cools to room temperature with the furnace simultaneously, takes out sample, obtains Fe-Si-B amorphous-copper laminar composite material.
Fe-Si-B amorphous through preparing the present embodiment-copper laminar composite material linkage interface is observed, and sample connects good, linkage interface is straight zero defect.
Embodiment three
The present embodiment is a kind of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.Described Fe-Si-B non-crystaline amorphous metal-copper laminar composite material is made up of one deck Fe-Si-B amorphous thin ribbon and two-layer copper, and described Fe-Si-B amorphous thin ribbon is clipped between described two-layer copper.
The Fe-Si-B amorphous thin ribbon that the present embodiment adopts is GB 1K101; The copper adopted is brass bar.
The present embodiment also proposed a kind of method preparing Fe-Si-B non-crystaline amorphous metal-copper laminar composite material, comprises the following steps:
Step 1, surface treatment; By the surface finish polishing to be connected of Fe-Si-B amorphous and brass, and after removing brass surfaces oxide with 5% watery hydrochloric acid, in ethanol with Ultrasonic Cleaning 1min respectively in acetone.
Step 2, precompressed.The Fe-Si-B amorphous handled well is placed between two pieces of copper rods, defines the sample of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material.Described sample is put into diffusion in vacuum jockey, and carries out precompressed by diffusion in vacuum jockey to sample pressurization, described moulding pressure is 5MPa.
Step 3, diffusion connects.Described diffusion connection is realized by diffusion in vacuum jockey, and detailed process is:
0.6 × 10 is evacuated to diffusion in vacuum jockey
-2after Pa, with the heating rate of 30 DEG C/min 500 DEG C be warming up to the sample being arranged in diffusion in vacuum jockey and be incubated.When the temperature of sample rises to 500 DEG C, to described sample pressurization 70MPa and pressurize; Insulation and dwell time are 20min.After insulation and pressurize terminate, unload be depressed into 2MPa to sample, sample cools to room temperature with the furnace simultaneously, takes out sample, obtains Fe-Si-B amorphous-copper laminar composite material.
Fe-Si-B amorphous through preparing the present embodiment-brass laminar composite linkage interface is observed, and sample connects good, linkage interface is straight zero defect.
Claims (1)
1. prepare the method for Fe-Si-B non-crystaline amorphous metal-copper laminar composite material for one kind, described Fe-Si-B non-crystaline amorphous metal-copper laminar composite material is made up of one deck Fe-Si-B amorphous thin ribbon and two-layer copper, and described Fe-Si-B amorphous thin ribbon is clipped between described two-layer copper; Described Fe-Si-B amorphous thin ribbon is GB 1K101; Described copper is fine copper rod or brass bar; It is characterized in that, its preparation process comprises the following steps:
Step 1, surface treatment; By the connecting surface sanding and polishing of Fe-Si-B amorphous and copper, and after removing copper surface oxide with 5% watery hydrochloric acid, in ethanol with Ultrasonic Cleaning 1min respectively in acetone, obtain the good Fe-Si-B non-crystaline amorphous metal of surface treatment and copper;
Step 2, precompressed; Fe-Si-B amorphous good for surface treatment is placed between two pieces of copper rods, defines the sample of Fe-Si-B non-crystaline amorphous metal-copper laminar composite material; Described sample is put into diffusion in vacuum jockey, and carries out precompressed by diffusion in vacuum jockey to sample pressurization, described moulding pressure is 5MPa;
Step 3, diffusion connects; The process that described diffusion connects is:
After diffusion in vacuum jockey is vacuumized, with the heating rate of 10 ~ 30 DEG C/min 480 ~ 500 DEG C be warming up to the sample being arranged in diffusion in vacuum jockey and be incubated; When the temperature of sample rises to 480 ~ 500 DEG C, to described sample pressurization 70 ~ 90MPa and pressurize; Insulation and dwell time are 20 ~ 40min; After insulation and pressurize terminate, to sample release, sample cools to room temperature with the furnace simultaneously, takes out sample, obtains Fe-Si-B amorphous-copper laminar composite material.
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| CN103895313B (en) * | 2014-03-14 | 2015-10-07 | 西北工业大学 | The preparation method of a kind of Fe-based amorphous alloy-copper multilayer composite board |
| CN108372211A (en) * | 2016-12-22 | 2018-08-07 | 中国航空制造技术研究院 | A kind of preparation method of amorphous enhancing alloy in lightweight composite protective material |
| CN106825887A (en) * | 2017-02-24 | 2017-06-13 | 东莞帕姆蒂昊宇液态金属有限公司 | A kind of joint method of amorphous alloy electronic product shell and middle plate |
| CN106939378B (en) * | 2017-03-10 | 2018-08-10 | 西京学院 | The preparation method of non-crystaline amorphous metal/fine copper laminar composite |
| CN113025912B (en) * | 2021-03-01 | 2022-07-19 | 西北工业大学重庆科创中心 | Iron-nickel-based hard magnetic material and preparation method thereof |
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| CN102191401A (en) * | 2011-04-08 | 2011-09-21 | 南昌大学 | Preparation method of amorphous-reinforced copper-based composite material |
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