CN103451579B - A kind of preparation method of fibrous texture composite material of molybdenum and copper - Google Patents
A kind of preparation method of fibrous texture composite material of molybdenum and copper Download PDFInfo
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- CN103451579B CN103451579B CN201310459329.XA CN201310459329A CN103451579B CN 103451579 B CN103451579 B CN 103451579B CN 201310459329 A CN201310459329 A CN 201310459329A CN 103451579 B CN103451579 B CN 103451579B
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- molybdenum
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Abstract
The present invention relates to a kind of fibrous texture composite material of molybdenum and copper and preparation method thereof, the weave construction dense uniform of this matrix material, present obvious fibrous texture feature, wherein the molybdenum content of molybdenum content according to weight percent is 55% ~ 90%, and all the other are copper.Molybdenum fiber is mixed with the fluffy two-dimensional fiber felt of appropriateness by paved, folded by preparation method; Fibrefelt is carried out mold pressing compacting and obtain three-dimensional fiber precast body, pressing pressure controls within the scope of 20-80MPa; Copper ingot is positioned over ZrO together with molybdenum fiber preform
2in sintering boat, copper is positioned over above molybdenum fiber preform, and under vacuum conditions, vacuum tightness remains on 1 × 10
-3more than Pa, at temperature is 1180 DEG C ~ 1350 DEG C, insulation 0.5h ~ 2h; Cool to less than 160 DEG C with the furnace to come out of the stove, by the rich copper removing on gained molybdenum-copper base surface, namely obtain the composite material of molybdenum and copper of fibrous texture.
Description
Technical field
The invention belongs to a kind of metallurgical technology field, relate to the preparation technology of matrix material, especially a kind of dense uniform, feature obvious fibrous texture tissue, molybdenum content is adjustable and composite material of molybdenum and copper of a wider range and preparation method thereof.
Background technology
Composite material of molybdenum and copper is by the specific function material of molybdenum, copper two kinds of monomer Homogeneous phase mixing.It combines the intrinsic physicals of molybdenum and copper, possesses good anti-melting welding, resistance to scaling loss and the performance such as hot strength, electric-conductivity heat-conductivity high, is thus widely used in the fields such as electronics, electric power, military affairs.
Molybdenum copper two kinds of elements neither dissolve each other and do not form intermetallic compound, and therefore, composite material of molybdenum and copper adopts the preparation of conventional powder metallurgical technique, mainly contains infiltration method, liquid phase activation sintering method.
Infiltration method comprises two kinds, and a kind of is the molybdenum skeleton suppressing molybdenum powder, sinter the certain porosity of formation, then on molybdenum skeleton, places oozed copper powder or copper base, makes copper melt and is infiltrated up to molybdenum skeleton, form composite material of molybdenum and copper under being placed in vacuum environment; The advantage of this technology is that the frame strength in product is higher, not easily loose, and shortcoming is that the closed pore always with minute quantity in pre-burning skeleton exists, and product is difficult to the high-compactness reaching more than 99%.Another kind is in molybdenum powder, be mixed with a certain amount of copper powder (copper powder ratio does not need to reach product requirement), and this powder mix is repressed, sintering forms skeleton, then oozes copper with aforesaid method, obtained composite material of molybdenum and copper; The advantage of this technology is that the skeleton in product can avoid closed pore to be formed, hole in molybdenum skeleton is selectively copper filled substantially, shortcoming is that the molybdenum content of product is difficult to improve, preparation is difficult to for size, product that shape is more complicated, simultaneously easily produce impurity and gas in product, make alloying element be difficult to be uniformly dispersed, compact structure, efficiency is lower, and the powder quality needed requires higher, manufacturing cost is high.
Liquid phase activation sintering method adopts the method for conventional liquid phase sintering process, i.e. mixed powder, compacting and sintering.On this basis, by adding the activating element of trace as cobalt, nickel etc. in pressed compact, sintering temperature is made to reduce thus.The advantage of this technology is the dimensional precision raising of product, and resistance to air loss improves, and shortcoming introduces new element in activated process, falls low-alloyed thermal conductivity and electroconductibility.
In addition, the process of compacting is had in both methods above-mentioned.Due to molybdenum, copper (molybdenum: 10.22g/cm
3, copper: 8.93g/cm
3) proportion difference less, is shaped more difficult, product easily exists void distribution inequality, be difficult to the problems such as densification completely.
Instant invention overcomes above-mentioned defect.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, provide that a kind of density is high, foreign matter content is low, uniform texture, molybdenum content are adjustable and composite material of molybdenum and copper of a wider range and preparation method thereof.
Above-mentioned purpose of the present invention is achieved by the following technical solutions:
A kind of fibrous texture composite material of molybdenum and copper, it is characterized in that the microscopic appearance of described fibrous texture composite material of molybdenum and copper is fibrous texture tissue, composition is (wt%): molybdenum content is 55% ~ 90%, and all the other are copper.
For the weight percent of above-mentioned molybdenum, can be 55,56,57,58,59,60,61,62,63,64,65,66,67,68,69,70,71,72,73,74,75,76,77,78,79,80,81,82,83,84,85,86,87,88,89 or 90%.
For the preparation method of above-mentioned fibrous texture composite material of molybdenum and copper, comprise the steps:
(1) be that the molybdenum fiber of 0.1 ~ 500 μm is mixed with the fluffy two-dimensional fiber felt of appropriateness by paved, folded by diameter, two-dimensional fiber felt mesoporosity rate is maximum reaches 90%;
(2) fibrefelt is carried out mold pressing compacting and obtain three-dimensional fiber precast body, pressing pressure controls within the scope of 20-80MPa;
(3) copper ingot is positioned over ZrO together with molybdenum fibre three-dimensional precast body
2in sintering boat, copper is positioned over above molybdenum fiber preform;
(4), under sintering boat being placed in vacuum environment, vacuum tightness remains on 1 × 10
-3more than Pa, heat temperature raising speed is 3 ~ 11 DEG C/min, and temperature is 1180 DEG C ~ 1350 DEG C, and soaking time is 0.5h ~ 2h;
(5) cool to less than 160 DEG C with the furnace to come out of the stove, by the rich copper removing on gained molybdenum-copper base surface, namely obtain the composite material of molybdenum and copper of fibrous texture.
On the basis of such scheme, in described step 2, the porosity of three-dimensional molybdenum fiber preform is 15%-34%, and the porosity for above-mentioned three-dimensional molybdenum fiber preform can be 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33% or 34%; In step 3, the weight of copper ingot is the 105%-120% according to filling molybdenum fiber preform porosity, and the weight of copper ingot can be according to filling 105%, 106% of molybdenum fiber preform porosity, 107%, 108%, 109%, 110%, 111%, 112%, 113%, 114%, 115%, 116%, 117%, 118%, 119% or 120%.
Because fibrefelt is after different pressing pressure compacting, the molybdenum fiber preform of different aperture degree can be formed, and porosity ranges is wider.Now, the apparent density of molybdenum fiber preform is 66% ~ 75%(of theoretical density and the porosity of molybdenum fiber preform is 15% ~ 34%), calculate 105% ~ 120% of porosity more subsequently and ooze copper amount accordingly, infiltration obtains the composite material of molybdenum and copper of dense uniform, the obvious fibrous texture tissue of feature after filling.
Compared to prior art, the present invention has the following advantages:
1. the hole of the molybdenum fiber preform prepared by the present invention is all communicating pores, and under vacuum conditions, communicating aperture space occupies without gas, is conducive to fully soaking into of copper phase, and the densification degree of composite material of molybdenum and copper is high;
2. the molybdenum fiber preform that prepared by the present invention can form the porosity of relative broad range, can keep certain porosity and aperture shape after high temperature sintering simultaneously, and the composite material of molybdenum and copper of acquisition allows the composition range of change large;
3. the composite material of molybdenum and copper prepared of the present invention weave construction dense uniform, present obvious fibrous texture feature; Avoid composite material of molybdenum and copper prepared by common process and there is void distribution inequality, be difficult to the phenomenons such as completely fine and close.
Accompanying drawing explanation
Fig. 1 be the present invention prepare molybdenum content 80wt%, copper content 20wt% the metallographic structure photo of fibrous texture composite material of molybdenum and copper
Fig. 2 is the local magnification region of Fig. 1.
Fig. 3 is longitudinal tissue's structure iron of fibrous texture composite material of molybdenum and copper prepared by the embodiment of the present invention 2, wherein molybdenum content 85wt%, copper content 15wt%.
Embodiment
Embodiment 1
For a kind of fibrous texture composite material of molybdenum and copper, wherein become to be grouped into and content is molybdenum 80wt%, copper 20wt%.Experiment adopts molybdenum Fibre diameter to be 20 μm, and purity >=99.9%, copper is T2 red copper.
Preparation technology comprises the following steps:
(1) molybdenum fiber is mixed with the fluffy two-dimensional fiber felt of appropriateness by paved, folded, fibrefelt mesoporosity rate is 80%;
(2) fibrefelt is carried out mold pressing compacting and obtain three-dimensional fiber precast body, pressing pressure controls within the scope of 20-50MPa, and now the porosity of fiber preform is 23% ~ 34%;
(3) copper ingot is positioned over ZrO together with molybdenum fiber preform
2in sintering boat, copper is positioned over above molybdenum fiber preform;
(4), under sintering boat being placed in vacuum environment, vacuum tightness remains on 1 × 10
-3more than Pa, heat temperature raising speed is 3 ~ 11 DEG C/min, and temperature is 1240 DEG C, and soaking time is 1.5h;
(5) cool to less than 160 DEG C with the furnace to come out of the stove, by the rich copper removing on gained molybdenum-copper base surface, namely obtain the composite material of molybdenum and copper of fibrous texture.Figure 1 shows that the structure figure of this fibrous texture composite material of molybdenum and copper, its grey area is molybdenum fiber, and yellow area is metallic copper; Figure 2 shows that the local magnification region of Fig. 1, as shown in Figure 2, in conjunction with tight, smooth, there is not heterogeneous phase in molybdenum fiber and copper interphase interface, its tissue topography keeps obvious fibrous texture feature; The density of composite material of molybdenum and copper is 99.71%.
Embodiment 2
A kind of fibrous texture composite material of molybdenum and copper, for become to be grouped into and content be molybdenum 85wt%, copper 15wt%.Experiment adopts molybdenum Fibre diameter to be 30 μm, and purity >=99.9%, copper is T2 red copper.
Preparation technology comprises the following steps:
(1) molybdenum fiber is mixed with the fluffy two-dimensional fiber felt of appropriateness by paved, folded, fibrefelt mesoporosity rate is 75%;
(2) fibrefelt is carried out mold pressing compacting and obtain three-dimensional fiber precast body, pressing pressure controls within the scope of 50-80MPa, and now the porosity of fiber preform is 15% ~ 22%;
(3) copper ingot is positioned over ZrO together with molybdenum fiber preform
2in sintering boat, copper is positioned over above molybdenum fiber preform;
(4), under sintering boat being placed in vacuum environment, vacuum tightness remains on 1 × 10
-3more than Pa, heat temperature raising speed is 3 ~ 11 DEG C/min, and temperature is 1270 DEG C, and soaking time is 1h;
(5) cool to less than 160 DEG C with the furnace to come out of the stove, by the rich copper removing on gained molybdenum-copper base surface, namely obtain the composite material of molybdenum and copper of fibrous texture.Figure 3 shows that longitudinal tissue's structure iron of this fibrous texture composite material of molybdenum and copper, the density of this material is 99.65%.
Claims (2)
1. a preparation method for fibrous texture composite material of molybdenum and copper, comprises the steps:
Molybdenum fiber is mixed with the fluffy two-dimensional fiber felt of appropriateness by paved, folded,
Two-dimensional fiber felt is carried out mold pressing compacting and obtain three-dimensional fiber precast body;
Copper ingot is positioned over ZrO together with molybdenum fiber preform
2in sintering boat, copper is positioned over above molybdenum fiber preform;
Carry out heat temperature raising under sintering boat being placed in vacuum environment and be incubated;
Cool to less than 160 DEG C with the furnace to come out of the stove, by the rich copper removing on gained molybdenum-copper base surface, complete the composite material of molybdenum and copper preparing fibrous texture, it is characterized in that:
Be that the molybdenum filament of 0.1 ~ 500 μm is mixed with the fluffy two-dimensional fiber felt of appropriateness by paved, folded by diameter, two-dimensional fiber felt is carried out mold pressing compacting and obtain three-dimensional fiber precast body, pressing pressure controls within the scope of 20-80MPa; Copper ingot is positioned over ZrO together with molybdenum fiber preform
2in sintering boat, copper is positioned over above molybdenum fiber preform; Under sintering boat is placed in vacuum environment, vacuum tightness remains on 1 × 10
-3more than Pa, heat temperature raising speed is 3-11 DEG C/min, and temperature is 1180 DEG C-1350 DEG C, after insulation 0.5-2h, cools to less than 160 DEG C with the furnace and comes out of the stove, and by the rich copper removing on gained molybdenum-copper base surface, completes the composite material of molybdenum and copper preparing fibrous texture;
The porosity of three-dimensional molybdenum fiber is 15% ~ 34%, and the weight of copper ingot is calculate according to fill molybdenum fiber preform porosity 105% ~ 120% to ooze copper amount accordingly, two-dimensional fiber felt mesoporosity rate maximum 90%;
The material of above-mentioned fibrous texture composite material of molybdenum and copper to be microscopic appearance be fibrous texture tissue, and be 55% ~ 90% according to the content that weight percent is molybdenum, all the other are copper.
2. according to the fibrous texture composite material of molybdenum and copper that method described in claim 1 prepares.
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| CN105543513A (en) * | 2015-12-19 | 2016-05-04 | 湖南科技大学 | Molybdenum-copper composite material in three-dimensional communicated reticular structure and preparation method of molybdenum-copper composite material |
| CN107740006B (en) * | 2017-09-19 | 2020-01-03 | 上海工程技术大学 | Cu/W composite material with anisotropic performance and preparation method thereof |
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