CN102344149B - Preparation method of ZrB2 powder material - Google Patents

Abstract

The invention relates to a preparation method of a ZrB2 powder material, which comprises the following steps: (1) preparing 38.66-43.04 wt% of Mg, 22.14-20.57 wt% of B2O3 and 39.19-36.40 wt% of ZrO2; (2) putting the weighed powder raw materials into a ball milling tank, and evenly mixing in a planetary ball mill; (3) putting the evenly mixed reaction materials in a die to obtain a round cake under the pressure of 10-60 MPa; putting the formed lump material into a reaction vessel, and putting a detonator on the bottom surface; charging 0.5-1.5 MPa argon gas into the reaction vessel at room temperature; heating, discharging the gas when the temperature of the reaction vessel rises to 180-200 DEG C, charging 1.5-5 MPa argon gas, and continuing heating; when the temperature in the reaction vessel reaches 250-300 DEG C, the detonator is combusted until all the material is reacted; and (4) carrying out furnace cooling on the product to room temperature under the argon shield, washing the prepared material with hydrochloric acid for 5-15 days, washing with distilled water, separating, and carrying out vacuum drying to obtain the ZrB2 powder material.

Description

A kind of ZrB 2The preparation method of powder body material

Technical field

The present invention relates to contain the preparation of Zr, B powder body material.

Background technology

ZrB ₂Being a kind of very potential special ceramic material, is the typical material of ultrahigh-temperature structural ceramics.ZrB ₂Pottery has fusing point height (3245 ℃), hardness high (22GPa), thermal conductivity and good conductivity (9.2 * 10 ^-6Ω), good with heat-shock resistance, the solid-state mutually characteristics such as stable of corrosion stability, in addition, also have good chemical stability, capture neutron, the special property such as fire-retardant, heat-resisting, corrosion-resistant and lightweight.Domestic to ZrB ₂Research mainly in the sixties in 20th century and the nineties in 20th century.Phase early 1960s was because the needs of China's nuclear industry and rocketry carried out ZrB ₂Research.The nineties in 20th century, in the refractory materialss such as the crucible lining of matrix material, high-temperature thermocouple protection tube, metallurgical metal and electrostatic coating material, all obtained application.Abroad to ZrB ₂Research carry out early and more deep.Except above several aspects, also obtain using more widely at aspects such as electrode materials, anticorrosive wear-resistant coating, cutting material and solar absorbing films.At present, mainly there are the shortcomings such as cost is high, purity is low in the magnesiothermic reduction boron preparation technology of use.

Summary of the invention

The purpose of this invention is to provide a kind of ZrB ₂The preparation method of powder body material.

The present invention is a kind of ZrB of preparation ₂The method of powder body material the steps include:

(1) by mass percentage Mg:38.66～43.04, B ₂O ₃: 22.14～20.57, ZrO ₂: 39.19～36.40 ratio is prepared burden;

(2) load weighted material powder is packed into ball grinder mixes in planetary ball mill, and Ball-milling Time is 8～24 hours, and rotating speed is 50～150r/min, and ratio of grinding media to material is 1: 2～1: 3, and ball-milling medium is Al ₂O ₃Ball;

(3) place mould under the pressure of 10～60MPa, to become round pie the reaction mass that mixes; The lumpy material of forming is put into reaction vessel, put detonator in its bottom surface; At room temperature, be filled with 0.5～1.5MPa argon gas in reaction vessel, final vacuum in 2 minutes is in the argon gas atmosphere protection reaction mass; Then heating, again exhaust when the temperature of reaction vessel is raised to 180～200 ℃, the argon gas that is filled with afterwards 1.5～5MPa continues heating; Detonator burning when temperature in the reaction vessel reaches 250 ℃～300 ℃, cause simultaneously the first layer material generation magnesium thermal response, discharge a large amount of heat, cut off heating power supply this moment, make the continuation reaction under the keeping of the large calorimetric that reaction is emitted of lower one deck material, until all material reaction is complete;

(4) resultant cools to room temperature with the furnace under argon shield, and the material of preparation at the salt acid elution 5～15 days that through over-richness is 8～11.6mol/L, and will be separated through distilled water wash after the washing at last, and vacuum-drying obtains ZrB ₂Powder body material, ZrB ₂Content is greater than 90～98%, granularity 1～10 μ m.

The invention has the beneficial effects as follows that Production Flow Chart is simple, energy consumption is low, the available low-cost higher ZrB of purity that obtains ₂Powder, and pollute littlely, be suitable for suitability for industrialized production.

Existing preparation method's two steps are simplified, and preparation flow is simple, is suitable for suitability for industrialized production.

Embodiment

Embodiment 1:

By mass percentage Mg:38.66, B ₂O ₃: 22.14, ZrO ₂: 39.19 take by weighing raw material powder; Then the stainless steel jar mill of load weighted material powder being packed into mixes in planetary ball mill, and Ball-milling Time is 8 hours, and rotating speed is 150r/min, and ratio of grinding media to material is 1: 2, and ball-milling medium is Al ₂O ₃Ball.Then the reaction mass that mixes is placed the mould of 250g under the pressure of 15MPa, to become round pie with pressing machine; The lumpy material of forming is put into reaction vessel, put detonator in its bottom surface; At room temperature, be filled with the 0.5MPa argon gas in reaction vessel, final vacuum in 2 minutes is in the argon gas atmosphere protection reaction mass; Then heating, again exhaust when the temperature of reaction vessel is raised to 200 ℃, the argon gas that is filled with afterwards 2MPa continues heating; Detonator burning when temperature in the reaction vessel reaches 298 ℃, cause simultaneously the first layer material generation magnesium thermal response, discharge a large amount of heat, cut off heating power supply this moment, make the continuation reaction under the keeping of the large calorimetric that reaction is emitted of lower one deck material, until all material reaction is complete.The material of preparation was being soaked 9 days through 11.6mol/L salt acid elution, and will separate at last through distilled water wash after the washing, vacuum-drying obtains the finished product.ZrB ₂Purity be 91.83%, granularity is between 1-3 μ m.

Embodiment 2:

By mass percentage Mg:40.92, B ₂O ₃: 21.33, ZrO ₂: 37.75 take by weighing raw material powder; Then the stainless steel jar mill of load weighted material powder being packed into mixes in planetary ball mill, and Ball-milling Time is 8 hours, and rotating speed is 150r/min, and ratio of grinding media to material is 1: 2, and ball-milling medium is Al ₂O ₃Ball.Then the reaction mass that mixes is placed the mould of 250g under the pressure of 15MPa, to become round pie with pressing machine; The lumpy material of forming is put into reaction vessel, put detonator in its bottom surface; At room temperature, be filled with the 0.5MPa argon gas in reaction vessel, final vacuum in 2 minutes is in the argon gas atmosphere protection reaction mass; Then heating, again exhaust when the temperature of reaction vessel is raised to 200 ℃, the argon gas that is filled with afterwards 2MPa continues heating; Detonator burning when temperature in the reaction vessel reaches 298 ℃, cause simultaneously the first layer material generation magnesium thermal response, discharge a large amount of heat, cut off heating power supply this moment, make the continuation reaction under the keeping of the large calorimetric that reaction is emitted of lower one deck material, until all material reaction is complete.The material of preparation was being soaked 9 days through 11.6mol/L salt acid elution, and will separate at last through distilled water wash after the washing, vacuum-drying obtains the finished product.ZrB ₂Purity be 94.35%, granularity is between 3-5 μ m.

Embodiment 3:

By mass percentage Mg:43.04, B ₂O ₃: 20.57, ZrO ₂: 36.40 take by weighing raw material powder; Then the stainless steel jar mill of load weighted material powder being packed into mixes in planetary ball mill, and Ball-milling Time is 8 hours, and rotating speed is 150r/min, and ratio of grinding media to material is 1: 2, and ball-milling medium is Al ₂O ₃Ball.Then the reaction mass that mixes is placed the mould of 250g under the pressure of 15MPa, to become round pie with pressing machine; The lumpy material of forming is put into reaction vessel, put detonator in its bottom surface; At room temperature, be filled with the 0.5MPa argon gas in reaction vessel, final vacuum in 2 minutes is in the argon gas atmosphere protection reaction mass; Then heating, again exhaust when the temperature of reaction vessel is raised to 200 ℃, the argon gas that is filled with afterwards 2MPa continues heating; Detonator burning when temperature in the reaction vessel reaches 298 ℃, cause simultaneously the first layer material generation magnesium thermal response, discharge a large amount of heat, cut off heating power supply this moment, make the continuation reaction under the keeping of the large calorimetric that reaction is emitted of lower one deck material, until all material reaction is complete.The material of preparation was being soaked 9 days through 11.6mol/L salt acid elution, and will separate at last through distilled water wash after the washing, vacuum-drying obtains the finished product.ZrB ₂Purity be 90.59%, granularity is between 5-7 μ m.

Claims (1)

1. one kind prepares ZrB ₂The method of powder body material the steps include:

(1) by mass percentage Mg:38.66～43.04, B ₂O ₃: 22.14～20.57, ZrO ₂: 39.19～36.40 ratio is prepared burden, and three's quality equals 100% than sum;

(2) load weighted material powder is packed into ball grinder mixes in planetary ball mill, and Ball-milling Time is 8～24 hours, and rotating speed is 50～150r/min, and ratio of grinding media to material is 1: 2～1: 3, and ball-milling medium is Al ₂O ₃Ball;

(3) place mould under the pressure of 10～60MPa, to become round pie the reaction mass that mixes; The lumpy material of forming is put into reaction vessel, put detonator in its bottom surface; At room temperature, be filled with 0.5～1.5MPa argon gas in reaction vessel, final vacuum in 2 minutes is in the argon gas atmosphere protection reaction mass; Then heating, again exhaust when the temperature of reaction vessel is raised to 180～200 ℃, the argon gas that is filled with afterwards 1.5～5MPa continues heating; Detonator burning when temperature in the reaction vessel reaches 250 ℃～300 ℃, cause simultaneously the first layer material generation magnesium thermal response, discharge a large amount of heat, cut off heating power supply this moment, make the continuation reaction under the keeping of the large calorimetric that reaction is emitted of lower one deck material, until all material reaction is complete;

(4) resultant cools to room temperature with the furnace under argon shield, and the material of preparation at the salt acid elution 5～15 days that through over-richness is 8～11.6mol/L, and will be separated through distilled water wash after the washing at last, and vacuum-drying obtains ZrB ₂Powder body material, ZrB ₂Content is greater than 90～98%, granularity 1～10 μ m.