CN102529217B - Method for preparing copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding - Google Patents
Method for preparing copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding Download PDFInfo
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Abstract
The invention discloses a method for preparing a copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding. In the copper/molybdenum composite board with molybdenum fibers, prepared by the method, molybdenum is fractured to be in a fibrous form by accumulative roll bonding, and then is pinned in a copper plate, and the density of molybdenum fiber can be controlled by accumulative roll bonding passes; and the preparation comprises pretreatment, hot rolling bonding, accumulative roll bonding, finished product annealing and follow-up processing. In the copper/molybdenum composite board with molybdenum fibers, prepared by the method, the copper/molybdenum composite board with different molybdenum fiber densities can be prepared by accumulative roll bonding, and during rolling, a copper-molybdenum interface does not crack, and has no oxidization phenomenon during heat treatment under an argon or hydrogen protective condition, and the prepared composite board has the advantages that the longitudinal tensile strength is 180-360MPa, the transverse tensile strength is 390-620MPa, the elongation rate is 25%-45% and the heat expansion coefficient is controllable. The method has the characteristics of simple preparation process, strong controllability and high yield, and has the most remarkable advantage of being used for large-scale production.
Description
Technical field
The present invention relates to the preparation of composite, particularly a kind of method of preparing copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding.
Background technology
Along with the development of the industrial technologies such as electronics, information, the energy, automobile, function metal-base composites more and more comes into one's own, and has a extensive future.This material require has the physical property such as higher mechanical property and high heat conduction, low-thermal-expansion, high connductivity.Copper/molybdenum structure composite plate possesses These characteristics, so be generally applied to electronic package material.Metal-base composites mainly contains the metal-base composites strengthened with high performance reinforcing fiber, whisker, particle etc.; The kinds such as the spontaneous reinforced composite of metallic matrix situ, laminate metal-base composites.Its manufacture method can be divided into: solid state fabrication techniques, liquid manufacturing technology and other manufacturing technologies.The method principal solid manufacturing technology of current manufactured copper/molybdenum composite plate, wherein the main complex method of rolling is, by carrying out surface treatment to sheet material, removing surface contamination layer, obtains clean surface, makes surface have certain roughness simultaneously, the plate surface with certain roughness is made to engage each other during rolling, formation preliminary mechanical combines, and makes phase counterdiffusion between interface metal simultaneously, strengthen interface bond strength further by annealing.
Preparation has good mechanics, the key of physical property molybdenum fiber copper/molybdenum composite plate makes molybdenum plate occur rupture and be pinned in composite plate by enough large roll-force, and its key technology mainly comprises: the operations such as surface treatment, aximal deformation value ply rolling and annealing.By surface treatment, surface contamination layer and oxide-film are cleaned out, obtain certain hardened layer, make that crack can occur in the operation of rolling and expose fresh metal, be beneficial to the engagement of metal between interface.Find the ply rolling technique of the preferably condition such as deflection, deformation velocity and deformation temperature.In annealing operation, find preferably annealing temperature and time, make the coupling mutually such as the release of molybdenum fiber and copper interface stress, the diffusivity improving element, materials microstructure state and continuous deformation ability, make interface have the transition zone of suitable thickness and form abundant and effective metallurgical binding, and make composite plate possess required microstructure and mechanical property.
The technology of preparing of copper/molybdenum composite plate is also relates in related documents and patent.Point out in american documentation literature (US4957823, US4950554, US4988392) that rolling compression bonding method prepares copper/molybdenum/copper composite plate; Zhu Aihui (Xi'an University of Architecture and Technology's Master's thesis, 2006) to propose containing the cold rolling of reagent coat for copper/molybdenum/copper composite plate, thinks to add one deck aluminium foil as transition zone between interface, composite plate can be made to reach and combine closely; Wang Haishan etc. are in document (Central South University's Master's thesis, 2004; Metal material heat treatment, 2004,29 (5); Rare metal, 2005,29 (1)) in, the research of some aspect has been carried out to copper/molybdenum/copper composite plate preparation technology and performance, proposed the impact on Interface composites quality and intensity of surface treatment mode, combination process and annealing schedule.Be and prepare laminated composite plate by rolling.
In view of above relevant copper/molybdenum composite plate technology of preparing data is visible, although some key technology has reached ripe, all not mentioned preparing copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding.So it is significant to prepare molybdenum fiber copper/molybdenum composite plate by the technique of surface treatment, aximal deformation value ply rolling and annealing, the method is simple, safety and economic.
Summary of the invention
The object of the invention is to, a kind of preparation method of molybdenum fiber copper/molybdenum composite plate is proposed, the method ordinary copper and molybdenum are as raw material, the feature of the molybdenum fiber composite plate of preparation is that after ply rolling, molybdenum plate fragments into threadiness, dispersion is pinned in copper coin, meets the demand of hyundai electronics packaging industrial to high strength, electric-conductivity heat-conductivity high material.
In order to realize above-mentioned task, the present invention takes following technical solution:
A method for preparing copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding, is characterized in that, follows these steps to carry out:
Step one, pretreatment:
Get technical pure molybdenum blank, under 1000 DEG C ~ 1350 DEG C conditions, be rolled into the molybdenum plate of 0.5mm ~ 2.5mm, and heat-treat;
Get the technical pure copper coin that thickness is 2mm ~ 6mm, annealing in process 0.5 hour ~ 1.5 hours under 600 DEG C of temperature conditions;
Step 2, carries out surface finish by the molybdenum plate after heat treatment and copper coin water mill bed respectively, makes roughness Ra≤7 ~ 8 μm on surface, and with the surface after acetone cleaning polishing, with gases at high pressure removing molybdenum plate and the greasy dirt on copper coin surface, oxide and impurity;
Step 3, by the copper coin after cleaning and molybdenum plate, is stacked together successively with the order of copper/molybdenum/copper, then it is fixed from one end and certain gradient of polishing, so that milling train is nipped;
Step 4, is placed in the heating furnace of argon gas or hydrogen shield by above-mentioned superimposed good material, to be incubated 20 minutes ~ 30 minutes at 750 DEG C ~ 850 DEG C temperature;
Step 5, taken out by the sheet material after heating and be rolled with the single pass reduction ratio of 60% ~ 70% immediately, rolling temperature is 750 DEG C ~ 850 DEG C, and now copper coin belongs to hot rolling;
Step 6, after rolling, part and burr are split in the generation limit first cut on sheet material, then are cut into equivalent two parts;
Step 7, then repeats the operation of step 2 to step 6, and carries out the accumulation ply rolling of 4 ~ 10 passages;
Step 8, is placed in the annealing furnace of argon gas or hydrogen shield by the sheet material after accumulation ply rolling, under 200 DEG C ~ 900 DEG C conditions, be incubated 30 ~ 120min, is then cooled to room temperature and takes out, namely make molybdenum fiber copper/molybdenum composite plate.
By the molybdenum fiber copper/molybdenum composite plate of said method gained, size as required carries out selection rolling or shearing.
The present invention adopts Roll-bonding, and because multi-pass ply rolling total deformation is comparatively large, copper is softer comparatively large relative to molybdenum distortion, and create tension and make molybdenum plate generation fracture behaviour, therefore, molybdenum breaks to form threadiness in vertical rolling direction.Copper and Mo can not only be made closely to be combined with each other, and to improve conduction, the performance such as heat conduction and coefficient of expansion controllability of composite board significantly.The molybdenum fiber copper/molybdenum composite plate endwise tensile strength of preparation is 180 ~ 360MPa, transverse tensile strength is 390 ~ 620MPa, percentage elongation is 25% ~ 45%.Have the advantages that preparation technology is simple, controllability is strong and yield rate is high, its great advantage can be used for large-scale production.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is fixed form;
Fig. 3 is the structural representation of the molybdenum fiber copper/molybdenum composite plate adopting method of the present invention to prepare.Wherein Fig. 3 (a) is along rolling direction structure, and Fig. 3 (b) is vertical rolling direction structure.
The present invention is described in further detail for the embodiment provided below in conjunction with inventor.
Detailed description of the invention
Further research through applicant shows, in copper/molybdenum composite plate, molybdenum fiber is pinned in copper, when thermal environment affects, copper can expand, now the molybdenum of low expansion plays main inhibition to composite plate change in size, but role is limited, therefore increases molybdenum fibre density and is conducive to alleviating this problem, namely increase ply rolling number of times, which improves the dimensional stability of material under thermal environment.Meanwhile, the thermal uniformity of composite plate can be made to strengthen.In addition, due to increasing of interface, the more effective expansion preventing crackle of meeting, improves fracture toughness and the damage tolerance performance of material.
Embodiment 1: the preparation of molybdenum fibre density less copper/molybdenum composite plate
See Fig. 1, the preparation of molybdenum fibre density less copper/molybdenum composite plate, specifically implement according to the following steps:
One, molybdenum plate and copper coin preparation
Get technical pure molybdenum blank, under 1000 DEG C ~ 1350 DEG C conditions, be rolled into the molybdenum plate of 0.5mm ~ 2.5mm, and heat-treat, cool with stove;
Get technical pure copper coin, the thickness of copper coin is: 2.0mm ~ 6.0mm, puts in the lehr, and under 600 DEG C of temperature conditions, annealing in process 1 hour, cools with stove;
The surface water mill bed of above-mentioned molybdenum plate and copper coin is polished, makes roughness Ra≤7 ~ 8 μm on its surface; And with the surface after acetone cleaning polishing, to remove the greasy dirt on molybdenum plate and copper coin surface, oxide and impurity, use gases at high pressure to dry up surface simultaneously.
Two, the copper coin after cleaning being dried up and molybdenum plate are stacked together (thickness of molybdenum plate is less than and equals copper plate thickness, as 1: 1: 1 or 2: 1: 2) with the order of copper/molybdenum/copper, and the gross thickness of superimposed rear sheet material is less than 15mm; It is fixed (rivet interlacement, 1 place in Fig. 2) from one end and certain gradient of polishing, general effect as shown in Figure 2 so that milling train is nipped;
Three, above-mentioned superimposed good material is placed in the heating furnace of the gas shield such as argon gas or hydrogen, to be incubated 20 minutes ~ 30 minutes at 750 DEG C ~ 850 DEG C temperature;
Four, taken out by the sheet material after heating and be rolled with the single pass reduction ratio of 60% ~ 70% immediately, rolling temperature is 750 ~ 850 DEG C, and now copper coin belongs to hot rolling.
Five, the sheet material after rolling is cut except part and burr are split in generation limit, be cut into equivalent two parts again, then to repeat in above-mentioned steps one sanding operation to the operation (end of will nipping when repeating step 2 is fixed and be fixed tail end) of step 5 simultaneously, and carry out the accumulation ply rolling of 4 ~ 7 passages;
Six, the sheet material after accumulation ply rolling is placed in the annealing furnace of argon gas/hydrogen shield; 200 DEG C ~ 900 DEG C, heat-treat under the condition of temperature retention time 30 ~ 120min; then be cooled to room temperature taking-up and carry out Performance Detection, namely make molybdenum fibre density less copper/molybdenum composite plate.
Embodiment 2: the preparation of molybdenum fibre density larger copper/molybdenum composite plate
The present embodiment is prepared according to the technique in example 1, difference is, in repetition step one, sanding operation is to the operation of step 5, needs the accumulation ply rolling carrying out 8 ~ 10 passages, then perform the heat treatment of step 6, namely obtain molybdenum fibre density larger copper/molybdenum composite plate.
After testing, copper/molybdenum composite plate endwise tensile strength that prepared by above-described embodiment is 180 ~ 360MPa, transverse tensile strength is 390 ~ 620MPa, percentage elongation is 25% ~ 45%.Size as required can carry out follow-up selection rolling or shearing.
Claims (1)
1. a method for preparing copper/molybdenum composite board with molybdenum fibers by accumulative roll bonding, is characterized in that, follows these steps to carry out:
Step one, pretreatment:
Get technical pure molybdenum blank, under 1000 DEG C ~ 1350 DEG C conditions, be rolled into the molybdenum plate of 0.5mm ~ 2.5mm, and heat-treat;
Get the technical pure copper coin that thickness is 2mm ~ 6mm, annealing in process 0.5 hour ~ 1.5 hours under 600 DEG C of temperature conditions;
Step 2, carries out surface finish by the molybdenum plate after heat treatment and copper coin water mill bed respectively, makes roughness Ra≤7 ~ 8 μm on surface, and with the surface after acetone cleaning polishing, with gases at high pressure removing molybdenum plate and the greasy dirt on copper coin surface, oxide and impurity;
Step 3, by the copper coin after cleaning and molybdenum plate, be stacked together successively with the order of copper/molybdenum/copper, the Thickness Ratio of copper/molybdenum/copper is 1:1:1 or 2:1:2, and the gross thickness of superimposed rear sheet material is less than 15mm; Then it is fixed from one end and certain gradient of polishing, so that milling train is nipped;
Step 4, is placed in the heating furnace of argon gas or hydrogen shield by above-mentioned superimposed good material, to be incubated 20 minutes ~ 30 minutes at 750 DEG C ~ 850 DEG C temperature;
Step 5, taken out by the sheet material after heating and be rolled with the single pass reduction ratio of 60% ~ 70% immediately, rolling temperature is 750 DEG C ~ 850 DEG C, and now copper coin belongs to hot rolling;
Step 6, after rolling, part and burr are split in the generation limit first cut on sheet material, then are cut into equivalent two parts;
Step 7, then repeats the operation of step 2 to step 6, and carries out the accumulation ply rolling of 4 ~ 10 passages;
Step 8, is placed in the annealing furnace of argon gas or hydrogen shield by the sheet material after accumulation ply rolling, under 200 DEG C ~ 900 DEG C conditions, be incubated 30 ~ 120min, is then cooled to room temperature and takes out, namely make molybdenum fiber copper/molybdenum composite plate.
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| CN107097899A (en) * | 2017-03-17 | 2017-08-29 | 银邦金属复合材料股份有限公司 | Hull transit joint, aluminum steel composite material and its production method |
| CN108724847A (en) * | 2018-04-16 | 2018-11-02 | 兰州理工大学 | A kind of composite board and preparation method thereof of aluminium sheet and titanium plate accumulation ply rolling |
| CN109647882A (en) * | 2018-08-14 | 2019-04-19 | 南京交通职业技术学院 | A kind of high-strength high-plastic nano-stack material and preparation method thereof |
| CN109290371B (en) * | 2018-11-08 | 2020-09-29 | 瓯锟科技温州有限公司 | Cold rolling manufacturing method of copper-aluminum composite plate strip |
| CN112296086B (en) * | 2019-07-26 | 2022-09-09 | 南京理工大学 | Accumulative roll-stacking method for preparing high-bonding-strength copper-chromium composite material |
| CN111229833B (en) * | 2020-02-08 | 2022-05-10 | 西北工业大学太仓长三角研究院 | Method for preparing laminated metal composite material by multilayer-cumulative pack rolling |
| CN113617840B (en) * | 2021-08-09 | 2023-04-07 | 长春工业大学 | Preparation method of multi-metal multilayer gradient composite material |
| CN113664063B (en) * | 2021-08-26 | 2023-10-13 | 西安航空学院 | Preparation method of copper-molybdenum-copper layered composite material |
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| CN1850436A (en) * | 2006-04-10 | 2006-10-25 | 安泰科技股份有限公司 | Method for preparing copper/molybdenum/copper electronic packaging composite material with special layer thickness proportion |
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