High energy ball milling process-containing preparation method for nanometer multi-element composite crystal grain growth inhibitor

Abstract

The invention provides a high energy ball milling process-containing preparation method for a nanometer multi-element composite crystal grain growth inhibitor. The chemical formula of the inhibitor is (V<x>,M1<1-x>)(C<y>,N<1-y>), wherein M1 is at least one selected from the group consisting of chromium, titanium, molybdenum, tantalum, niobium and zirconium, x is more than 0.5 and no more than 0.95, and y is no less than 0.1 and no more than 0.9; or the chemical formula of the inhibitor is (Cr<x>,M2<1-x>)2(C<y>,N<1-y>), wherein M2 is at least one selected from the group consisting of vanadium, titanium, molybdenum, tantalum, niobium and zirconium, x is more than 0.5 and no more than 0.95, and y is no less than 0.1 and no more than 0.9. The preparation method comprises the following steps: (1) batching; (2) high energy ball milling: a step of dry grinding raw materials batched in the step (1) with a high energy ball mill at a rotating speed of 350 to 700 rpm so as to obtain ball milling powder; and (3) sintering. The method provided by the invention can reduce sintering temperature, shorten a production period and lower down requirements on granularity of the raw materials.

Description

technical field [0001] The invention belongs to the field of hard alloy preparation, and in particular relates to a multi-element compound grain growth inhibitor used in the preparation process of hard materials such as hard alloy and a preparation method thereof. Background technique [0002] Cemented carbide refers to a type of composite material prepared by powder metallurgy with carbide as the hard phase and iron, cobalt, nickel, etc. as the main component. A series of characteristics such as abrasiveness, excellent red hardness and thermal conductivity, etc., are suitable for making cutting tools, molds, grinding tools and other products. When preparing cemented carbide by powder metallurgy, the alloy compact must undergo solid-phase sintering and liquid-phase sintering. In these two sintering stages, the grains of the hard phase continue to grow, especially in the liquid phase sintering stage, the growth of the grains is particularly obvious, and it is easy to grow un...

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Problems solved by technology

However, the above method has the problems of high sintering temperature (1250-1500°C), long sintering time (1-4 hours), high energy consumption, and high cost.

Patent application 201310303214.1 discloses "a method for preparing a nano-multi-component composite grain growth inhibitor", and proposes to prepare a nano-multi-component composite grain growth inhibitor through an aqueous solution-precursor method combined with warm carbothermal reduction and nitriding treatment. Although it can reduce the sintering temperature (950-1400°C) and sintering time (1-2 hours) to a certain extent, and shorten the production cycle, it has the following problems: 1. The sintering temperature is still relatively high; 2. The required raw materials (except (except nitrogen) must be soluble or nano-scale powder, the raw material selection is narrow and the cost is high; 3, this method needs to use a large amount of water in the process of preparing solution or suspension, and produces a large amount of waste gas when spray drying, which is not necessary Conducive to environmental protection

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