CN105624443A - Preparation method for ultra-thin Al2O3 dispersion strengthened copper materials - Google Patents

Abstract

The invention provides a preparation method for ultra-thin Al2O3 dispersion strengthened copper materials and belongs to the field of preparation of metal materials. The ultra-thin Al2O3 dispersion strengthened copper materials prepared by the method have a small particle size and good high-temperature thermal stability, so that the problems that an existing preparation method is not likely to control the oxygen content needed in a reaction, the production cost is high and Al2O3 particles of prepared Al2O3 dispersion strengthened copper are large generally are solved. The method integrates the sol-gel method and hot pressed sintering, and the ultra-thin Al2O3 dispersion strengthened copper is prepared with Al(NO3)3, ammonium hydroxide and copper powder as raw materials. The preparation process of the preparation method is easy to control and cost is low; the size of the Al2O3 particles of the prepared ultra-thin Al2O3 dispersion strengthened copper is small, the performance of the copper materials changes little after annealing is carried out and the copper materials have excellent high-temperature thermal stability.

Description

A kind of ultra-fine Al2O3Dispersion-strengthened Cu material preparation method

Technical field

The invention belongs to field of metal preparation.

Background technology

Ultra-fine Al₂O₃Dispersion-strengthened Cu has high intensity, high conductivity and high thermal conductivity, and its properties all changes less when high temperature long-term work, namely the high high-temp stability of material is good, can be widely used for manufacturing metallurgical industry and the electronics industry such as resistance welding electrode, lead-in wire, commutator, relay copper sheet, prepared by dispersion-strengthened Cu it is crucial that how to introduce the Al of Dispersed precipitate in cuprio₂O₃Granule, what application was more at present is internal oxidation, but reacts required oxygen content in internal oxidation technical process and be difficult to control to, and production cost is expensive, other Al prepared such as mechanical mixing, co-electrodeposition method and nitrate fusion method₂O₃Dispersion-strengthened Cu, its Al₂O₃Granule is generally relatively larger (more than 2 ��m), thus affecting its superiority.

Summary of the invention

It is an object of the invention to provide that a kind of process is easily controlled, cost is low, Al in finished product₂O₃The ultra-fine Al that particle size is little, high high-temp stability is a lot of₂O₃Dispersion-strengthened Cu preparation method.

The present invention is achieved by the following technical programs: a kind of ultra-fine Al₂O₃Dispersion-strengthened Cu material preparation method, takes Al(NO₃)₃Add distilled water and prepare aluminum nitrate aqueous solution, ammonia is added in the aluminum nitrate aqueous solution being stirred vigorously to pH=9, obtains milky Al(OH)₃Colloidal sol, is slowly added to colloidal sol, stirring, standing, filtration by copper powder, obtain the mixture of copper and aluminium hydroxide wet gel, this mixture is put in ball mill and carry out wet-milling ball-milling treatment, be at room temperature loaded in graphite jig to carry out hot pressed sintering after dry 24h, sintering temperature 950 DEG C, pressure 45MPa, is incubated 2h, then carries out cold forging pressure, ratio of forging reduction 1:1, finally it is annealed processing, annealing temperature 900 DEG C, obtains finished product.

Described ammonia adds and adds colloidal dispersant polyethylene in aluminum nitrate aqueous solution process.

Described wet-milling Ball-milling Time is 4��5h.

There is advantages that

Preparation method process of the present invention is easily controlled, cost is low, Al in finished product₂O₃Content is 2.7%, Al in material after annealing₂O₃Average particle size particle size be 0.1 ��m, grain spacing 0.3 ��m, reach the level of super-refinement, after annealing, performance change is little, has good high high-temp stability.

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention will be further described.

Specific embodiment: the method for the invention adopts the preparation method that sol-gel process and hot pressed sintering combine, and takes Al(NO₃)₃Add distilled water and prepare aluminum nitrate aqueous solution, ammonia is added in the aluminum nitrate aqueous solution that is stirred vigorously to pH=9, is equivalent to 2.7%(volume fraction) Al₂O₃, for preventing the cohesion of colloidal particle, add colloidal dispersant polyvinyl alcohol, react for Al(NO₃)₃+3NH₄OH Al(OH)₃+3NH₄NO₃, obtain milky Al(OH)₃Colloidal sol, is slowly added to colloidal sol (purity 99.3%, granularity is less than 56 ��m) by copper powder, stirring, standing, filtration, obtain the mixture of copper and aluminium hydroxide wet gel, put into by this mixture in ball mill and carry out wet-milling ball milling 4��5h, at room temperature it is loaded in graphite jig to carry out hot pressed sintering, sintering temperature 950 DEG C, pressure 45MPa after dry 24h, insulation 2h, cold working adopts cold forging pressure, ratio of forging reduction 1:1, is finally annealed processing, annealing temperature 900 DEG C, obtains finished product.

With the thing phase morphology of Scanning Tunneling Microscopy finished product, Al₂O₃Granule is thin and is uniformly distributed, and after annealing, granule is not grown up, and recrystallization does not occur in matrix copper, has significantly high heat stability. Al in finished product₂O₃Content is 2.7%, Al after annealing₂O₃Average particle size particle size be 0.1 ��m, grain spacing 0.3 ��m, reach the crystal of super-refinement, after annealing, changes in material properties is little, has good high high-temp stability.

Preparation method process described in the embodiment of the present invention is easily controlled, cost is low, the ultra-fine Al of preparation₂O₃Dispersion-strengthened Cu, its Al₂O₃Particle size is little, and after annealing, changes in material properties is little, has good high high-temp stability.

Above content is the further description present invention done in conjunction with specific embodiment, it is impossible to assert that specific embodiment of the invention is confined to these explanations. For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, it is also possible to make some simple deduction or replace, protection scope of the present invention all should be considered as belonging to.

Claims (3)

1. a ultra-fine Al₂O₃Dispersion-strengthened Cu material preparation method, it is characterised in that: take Al(NO₃)₃Add distilled water and prepare aluminum nitrate aqueous solution, ammonia is added in the aluminum nitrate aqueous solution being stirred vigorously to pH=9, obtains milky Al(OH)₃Colloidal sol, is slowly added to colloidal sol, stirring, standing, filtration by copper powder, obtain the mixture of copper and aluminium hydroxide wet gel, this mixture is put in ball mill and carry out wet-milling ball-milling treatment, be at room temperature loaded in graphite jig to carry out hot pressed sintering after dry 24h, sintering temperature 950 DEG C, pressure 45MPa, is incubated 2h, then carries out cold forging pressure, ratio of forging reduction 1:1, finally it is annealed processing, annealing temperature 900 DEG C, obtains finished product.

2. preparation method as claimed in claim 1, it is characterised in that: described ammonia adds and adds colloidal dispersant polyethylene in aluminum nitrate aqueous solution process.

3. preparation method as claimed in claim 1, it is characterised in that: described wet-milling Ball-milling Time is 4��5h.