CN113441715B - Boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder and preparation method thereof - Google Patents

Boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder and preparation method thereof Download PDF

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CN113441715B
CN113441715B CN202110734749.9A CN202110734749A CN113441715B CN 113441715 B CN113441715 B CN 113441715B CN 202110734749 A CN202110734749 A CN 202110734749A CN 113441715 B CN113441715 B CN 113441715B
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powder
boron
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ultrafine
doped ultrafine
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CN113441715A (en
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张厚安
麻季冬
党伟
杨益航
古思勇
廉冀琼
陈超贤
马璐
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Xiamen University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/15—Carbonitride

Abstract

The invention provides a boron doped superfine powder(Ti, W, mo, nb, ta) (C, N) powder and a preparation method thereof, wherein the preparation method comprises the following steps: will H 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And ball milling and mixing with carbon black to obtain mixed powder. And then carrying out carbothermal reduction nitridation reaction on the mixed powder to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder. The invention can not only purify the grain boundary but also respectively react with excessive free carbon and nitrogen to generate BC or BN by adding excessive boron element in the raw material, thereby playing the toughening effect of the second phase particles. The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder prepared by the invention is ultrafine solid solution powder, which is the precondition for preparing high-performance B-doped ultrafine crystal (Ti, W, mo, nb, ta) (C, N) -Co-Ni cermet.

Description

Boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder and preparation method thereof
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder and a preparation method thereof.
Background
Cemented carbide is known as a tooth in the modern industry and is widely used in the fields of aerospace, aviation, automobiles, high-speed trains, shipbuilding, petroleum drilling, mine tools, military industry and the like. With the development of modern manufacturing industry, the use of difficult-to-process materials with high hardness, severe work hardening tendency and low heat conductivity is increasingly used, so that the working environment faced by the cutter is more complex, and the cutter material is required to have comprehensive properties of high hardness, high strength, high toughness, high wear resistance and the like. Titanium carbonitride (Ti (C, N)) base cermets were a tool material developed in the beginning of the 70 th century, with Ti (C, N) as the primary hard phase and nickel and cobalt as the primary binder phase. It has significant advantages over WC-based cemented carbides commonly used in current manufacturing industries. Firstly, the alloy has the advantages of high hardness (33 GPa, the hardness of the traditional hard alloy is less than or equal to 24 GPa), higher specific stiffness, red hardness, wear resistance, crater wear resistance, high-temperature chemical stability, lower friction coefficient and the like, and is particularly suitable for semi-finishing and finishing of high-speed steel and cast iron. Second, it contains no or little scarce strategic resources W and Co, and can reduce production costs by about 45-65%. It has been reported that in developed countries, the Ti (C, N) -based cermet is used as a tool material in a proportion of about 1/5 to 1/4 of the total tool material, up to 30% in japan, and its future demand will be 50% of the total indexable insert. Therefore, ti (C, N) -based cermet has become an ideal substitute material for WC-based hard alloy, and has very wide application prospect.
However, compared with WC-based hard alloy, ti (C, N) -based metal ceramic has high hardness and high wear resistance, but has lower strength and toughness, and is difficult to meet the performance requirements of the development of the modern manufacturing industry on cutter materials, so that the application of the Ti (C, N) -based metal ceramic is greatly limited. Currently, the existing approach to solve the problem of insufficient toughness of Ti (C, N) -based cermets is to prepare gradient Ti (C, N) coating materials on the surface of a metal matrix (such as hard alloy or high-speed steel) with lower hardness and better toughness by adopting a physical or chemical vapor deposition (PVD or CVD) technology. The Ti (C, N) coating cutter prepared by the method combines the high strength and high toughness of the metal matrix with the high hardness and wear resistance of the Ti (C, N) coating, thereby having better cutting performance. However, ti (C, N) -coated tools suffer from two distinct inherent disadvantages compared to Ti (C, N) -based cermet tools: first, because of the difference in composition, structure and thermal expansion coefficient between the Ti (C, N) coating and the substrate, cracks are easily generated on the surface of the coating and spread to the inside, resulting in failure of the coated tool. Secondly, in order to reduce the internal stress of the cutting edge of the coated cutting tool, the cutting edge must be passivated before coating, so that the Ti (C, N) coated cutting tool is not suitable for finish machining. Therefore, the Ti (C, N) -based metal ceramic tool cannot be replaced in the aspects of machining precision, machining efficiency, service life, application range and the like of the Ti (C, N) -based metal ceramic tool.
Disclosure of Invention
The invention aims to provide boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder which is ultrafine solid solution powder and has higher hardness and bending strength.
Another object of the present invention is to provide a method for preparing boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, which is simple to operate and easy to control various parameters, and is suitable for industrial mass production.
The invention solves the technical problems by adopting the following technical scheme.
The invention provides a preparation method of boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, which comprises the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 Mixing with carbon black ball milling for 3.5-4.5 h to obtain mixed powder;
s2, performing carbothermal reduction nitridation reaction on the mixed powder to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
The invention provides boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, which is prepared according to the preparation method.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder and the preparation method thereof have the beneficial effects that:
the invention uses H 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And mixing with carbon black, and performing carbothermal reduction nitridation reaction to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder. The powder is superfine solid solution powder, which is a precondition for preparing high-performance B-doped superfine crystal (Ti, W, mo, nb, ta) (C, N) -Co-Ni cermet.
The invention can not only purify the grain boundary but also respectively react with excessive free carbon and nitrogen to generate BC or BN in situ by adding proper excessive B element into the raw material, thereby playing the toughening effect of the second phase particles.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM image of boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder of example 1 of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder and the preparation method thereof according to the embodiment of the invention are described in detail below.
The embodiment of the invention provides a preparation method of boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, which comprises the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And mixing with carbon black for 3.5-4.5 h to obtain mixed powder. The addition of a proper excess of B element to the raw material not only can clean the grain boundary, but also can react with the excess free carbon and nitrogen in situ to generate BC or BN, respectively, thereby exerting the toughening effect of the second phase particles.
Further, in the preferred embodiment of the present invention, tiO 2 Carbon black, WO 3 、MoO 3 、Nb 2 O 5 And Ta 2 O 5 The weight ratio of (2) to (4) is 10-15:4-8:2-4:1-20.8-1.2:1. More preferably, tiO 2 Carbon black, WO 3 、MoO 3 、Nb 2 O 5 And Ta 2 O 5 The weight ratio of (2) is 12.5:6.25:3:1.25:1:1.
Further, in a preferred embodiment of the present invention, in the mixed powder, the H 3 BO 3 The weight percentage of the (B) is 0.1-3%.
S2, performing carbothermal reduction nitridation reaction on the mixed powder to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
Further, in the preferred embodiment of the present invention, the temperature of the carbothermal reduction nitridation reaction is 1300-1800 ℃, the reaction time is 1-3 hours, and the nitrogen partial pressure is 1-3 kPa.
The invention also provides boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, which is prepared according to the preparation method.
Further, in a preferred embodiment of the present invention, the boron doped ultra-fine (Ti, W, mo, nb, ta) (C, N) powder is an ultra-fine solid solution powder.
The invention adds proper excessive B element into the raw material, and prepares boron doped superfine (Ti, W, mo, nb, ta) (C, N) powder through carbothermic reduction nitridation reaction. Wherein, the B element can clean grain boundary and exert the toughening effect of the second phase particles. The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder is an ultrafine solid solution powder, is a precondition for preparing B-doped ultrafine-grained (Ti, W, mo, nb, ta) (C, N) -Co-Ni cermet and (Ti, W, mo, nb, ta) (C, N) -Co-Ni cermet with a double-grain structure, and is also a guarantee for realizing uniform dispersion of Co and Ni in the Ti (C, N) cermet.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder provided in the embodiment is prepared according to the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 Mixing with carbon black ball milling for 4 hours to obtain a mixtureMixing the powder. Wherein, tiO 2 Carbon black, WO 3 、MoO 3 、Nb 2 O 5 And Ta 2 O 5 The weight ratio of (2) is 12.5:6.25:3:1.25:1:1. In the mixed powder, H 3 BO 3 The weight percentage of (2) is 3%.
S2, heating the mixed powder to 1300 ℃ under the nitrogen partial pressure of 3kPa, and reacting for 3 hours to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder prepared in this example was measured for hardness on a small-load Vickers hardness tester and for flexural strength on an electronic universal material tester, respectively, and had a hardness of 92.5HRA and a flexural strength of 1600MPa.
Example 2
In this example, a boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder is provided, which is prepared according to the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And ball milling with carbon black for 4 hours to obtain mixed powder. Wherein, tiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And carbon black at a weight ratio of 12.5:6.25:3:1.25:1:1. In the mixed powder, H 3 BO 3 Is 0.1% by weight.
S2, heating the mixed powder to 1800 ℃ under the nitrogen partial pressure of 3kPa, and reacting for 3 hours to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder prepared in this example was measured for hardness on a small-load Vickers hardness tester and bending strength on an electronic universal material tester, respectively, and had a hardness of 92.9HRA and a bending strength of 1632MPa.
Example 3
In this example, a boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder is provided, which is prepared according to the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And ball milling with carbon black for 4 hours to obtain mixed powder. Wherein, tiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And carbon black at a weight ratio of 12.5:6.25:3:1.25:1:1. In the mixed powder, H 3 BO 3 The weight percentage of (2) is 3%.
S2, heating the mixed powder to 1800 ℃ under the nitrogen partial pressure of 3kPa, and reacting for 1h to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder prepared in this example was measured for hardness on a small-load Vickers hardness tester and for flexural strength on an electronic universal material tester, respectively, and had a hardness of 93.7HRA and flexural strength of 1720MPa.
Example 4
In this example, a boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder is provided, which is prepared according to the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And ball milling with carbon black for 4 hours to obtain mixed powder. Wherein, tiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And carbon black at a weight ratio of 12.5:6.25:3:1.25:1:1. In the mixed powder, H 3 BO 3 The weight percentage of (2) is 3%.
S2, heating the mixed powder to 1800 ℃ under the nitrogen partial pressure of 1kPa, and reacting for 3 hours to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder prepared in this example was measured for hardness on a small-load Vickers hardness tester and for flexural strength on an electronic universal material tester, respectively, and had a hardness of 93HRA and a flexural strength of 1686MPa.
Example 5
In this example, a boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder is provided, which is prepared according to the following steps:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And ball milling with carbon black for 4 hours to obtain mixed powder. Wherein, tiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And carbon black at a weight ratio of 12.5:6.25:3:1.25:1:1. In the mixed powder, H 3 BO 3 The weight percentage of (2%).
S2, heating the mixed powder to 1500 ℃ under the nitrogen partial pressure of 3kPa, and reacting for 2.5 hours to obtain boron-doped superfine (Ti, W, mo, nb, ta) (C, N) powder.
The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder prepared in this example was measured for hardness on a small-load Vickers hardness tester and for flexural strength on an electronic universal material tester, respectively, and had a hardness of 93.2HRA and a flexural strength of 1700MPa.
Test example 1
Boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powders were measured using a scanning electron microscope. An SEM image of the boron doped ultra fine (Ti, W, mo, nb, ta) (C, N) powder provided in example 1 is shown in fig. 1. As can be seen from FIG. 1, the boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder has a fine particle size and an average size of 200nm.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (5)

1. A method for preparing boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, comprising the steps of:
s1, H is 3 BO 3 、TiO 2 、WO 3 、MoO 3 、Nb 2 O 5 、Ta 2 O 5 And carbon black ball milling by 3.5 to the whole range4.5h mixing to obtain mixed powder; wherein, in the mixed powder, the H 3 BO 3 The weight percentage of the (B) is 0.1-3%;
s2, performing carbothermal reduction nitridation reaction on the mixed powder to obtain boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder.
2. The method according to claim 1, wherein in step S1, the TiO is obtained by 2 Said carbon black, said WO 3 Said MoO 3 The Nb is 2 O 5 And the Ta 2 O 5 The weight ratio of (2) to (1) is 10-15:4-8:2-4:1-2:0.8-1.2:1.
3. The method according to claim 1, wherein in the step S2, the carbothermal reduction nitridation reaction is performed at a temperature of 1300 to 1800 ℃ for a reaction time of 1 to 3 hours and a nitrogen partial pressure of 1 to 3kPa.
4. Boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder, characterized by being produced according to the production method as claimed in any one of claims 1 to 3.
5. The boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder of claim 4, wherein the boron-doped ultrafine (Ti, W, mo, nb, ta) (C, N) powder is an ultrafine solid solution powder.
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