CN109136605B - Self-propagating synthesis of copper-based composite powder and application thereof - Google Patents
Self-propagating synthesis of copper-based composite powder and application thereof Download PDFInfo
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- CN109136605B CN109136605B CN201710501432.4A CN201710501432A CN109136605B CN 109136605 B CN109136605 B CN 109136605B CN 201710501432 A CN201710501432 A CN 201710501432A CN 109136605 B CN109136605 B CN 109136605B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
The invention relates to a self-propagating synthesis of copper-based composite powder and application thereof, which is prepared by taking titanium powder, boron nitride powder, copper powder or/and copper-based alloy powder as raw materials, uniformly mixing the raw materials and then adopting self-propagating sintering; the mass fraction of the titanium powder in the raw materials is 15-50%, the mass fraction of the boron nitride powder is 5-20%, and the mass fraction of the copper powder or/and the copper-based alloy powder is 80-30% based on 100% of the total mass of the raw materials. Compared with the prior art, the copper-based composite powder provided by the invention comprises TiB2the/TiN binary ceramic reinforced phase and the BN lubricating phase can be used for preparing reinforced self-lubricating copper-based composite material and have TiB function2High hardness and high wear resistance of TiN, and high thermal conductivity of pure copper or copper-based alloy.
Description
Technical Field
The invention relates to copper-based composite powder and a preparation method thereof, in particular to copper-based composite powder containing TiB2Self-propagating synthesis and application of composite powder of a/TiN binary ceramic phase, a BN lubricating phase and a Cu (or Cu alloy) metal phase.
Background
Copper and its alloy material have excellent electric conduction, heat-conducting property, generally as friction part, heat dissipation part, conductive part widely apply to various machinery, electric power, etc. system. However, their low hardness, high density, poor wear resistance at high temperature and high speed conditions, and the like, have limited their use in high performance automobiles, airplanes, high speed trains, and advanced weaponry systems. Ceramic phase reinforced copper-based composite materials (CMMCs) are prepared by taking ceramic (particles, short fibers and continuous long fibers) as a reinforcing phase and taking copper and copper alloy as a matrix, and have comprehensive properties of metal and nonmetal. The composite material generally keeps good heat conduction and electric conduction performance of the copper alloy material, has higher hardness and strength, better corrosion resistance, more excellent wear resistance and relatively lower density and thermal expansion coefficient compared with the traditional copper alloy, and is an ideal choice for replacing the traditional copper alloy material.
Titanium diboride (TiB)2) The copper-based composite material is a ceramic material with high strength, high hardness and high Young modulus, has good electrical conductivity, is an ideal reinforcing phase of the copper-based composite material, and can keep the material to have higher electrical conductivity on the basis of improving the mechanical property and the wear-resisting property of the material. In addition, since TiB2Has a lower density and can contribute to weight reduction of parts. Titanium nitride (TiN) is a ceramic material with excellent mechanical and wear-resisting properties, has good electric conductivity, heat conductivity, high temperature resistance and chemical stability, has good interface bonding performance with metal materials, and is widely applied to a reinforcing phase of a hard alloy material.
Currently, TiB2And TiN have been gradually developed as reinforcing phases for copper-based composites. The patent number CN102828060B discloses a titanium nitride ceramic reinforced copper-based composite material and a preparation method thereof, wherein the raw materials comprise titanium nitride, titanium oxide, a sintering aid and carbon black according to the weight ratio, wherein a copper alloy is added into a preform, and the preparation method comprises the steps of heating, heat preservation, sintering and flowing nitrogen gas introduction, so that a porous titanium nitride preform with the porosity of 45-75% is obtained; preheating a die casting machine, and simultaneously heating the copper alloy to a molten state; pouring the molten copper alloy liquid into a die cavity for placing a prefabricated part, and pressing the molten copper alloy liquid into a die cavity by a pressAnd in the hole titanium nitride preform, after the ingot is cooled, separating the ingot from the die, and performing heat treatment to obtain the titanium nitride reinforced copper-based composite material. The patent number CN105220000A discloses a high-strength titanium diboride particle reinforced copper-based composite material and a preparation method thereof, wherein the high-strength titanium diboride particle reinforced copper-based composite material consists of the following components in percentage by volume: 6-9% of high-purity titanium diboride with purity of more than 98%, and copper alloy ZCuSn5Zn5Pb5And the content of the titanium diboride particles is 91-94%, and the high-strength titanium diboride particle reinforced copper-based composite material is obtained through the steps of smelting, stirring, heat preservation, casting and the like.
All the above works are with TiB2Or TiN particles are used as raw materials, and the density of the material is uneven and the performance of the composite material is influenced due to the difference of the particle density and the agglomeration of ceramic particles in the material mixing process. Although the method adopting the ceramic prefabricated block can avoid the influence of agglomeration of ceramic particles, the method needs to prepare the ceramic prefabricated block, and has more complex process and equipment and higher cost, thereby having greater limitation on large-scale production.
Disclosure of Invention
The invention provides a method for self-propagating synthesis of copper-based composite powder, which is prepared by uniformly mixing titanium powder, boron nitride powder, copper powder or/and copper-based alloy powder as raw materials and then adopting self-propagating sintering, wherein the method is based on powder preparation and aims at solving the problems in the prior art;
the mass fraction of the titanium powder in the raw materials is 15-50%, the mass fraction of the boron nitride powder is 5-20%, and the mass fraction of the copper powder or/and the copper-based alloy powder is 80-30% based on 100% of the total mass of the raw materials.
The invention takes titanium powder, boron nitride powder, copper powder or/and copper-based alloy powder as raw materials, wherein the titanium powder and the boron nitride powder in the raw materials react in the self-propagating sintering process: 3Ti +2BN → 2TiN + TiB2Namely, BN powder and Ti powder generate ceramic reinforced phase TiN + TiB through self-propagating2Not only avoid directly adopting TiB2Or TiN particles are used as the ceramic reinforcing phase, and the process and the equipment are simple, so that the preparation cost is saved. Furthermore, 3Ti +2BN → 2TiN + T according to the above reactioniB2: if the Ti powder is excessive in the self-propagating reaction process, BN is completely and basically reacted. The excess Ti powder may exist in the form of a Ti phase and may also form a new alloy phase with the Cu-based alloy. If the BN is excessive, the titanium powder is completely reacted and the BN phase remains, and the remaining BN can also be used as a self-lubricating medium to exist in the copper-based composite powder.
The method for self-propagating synthesis of copper-based composite powder provided by the invention takes titanium powder, boron nitride powder, copper powder or/and copper-based alloy powder as raw materials, the titanium powder, the boron nitride powder, the copper powder or/and the copper-based alloy powder are uniformly mixed and then are prepared by self-propagating sintering, ceramic prefabricated blocks do not need to be prepared, the process is simple, and TiB can be avoided2Or TiN particles as raw materials, due to the difference of particle density and the agglomeration problem of ceramic particles in the mixing process. The prepared material phase composition comprises TiB besides Cu (and/or copper-based alloy)2And TiN. Preferably, the main constituent phase of the material is TiB2TiN, BN, Cu (and/or copper-based alloys). More preferably, the material comprises 30-80.6% of Cu and/or copper-based alloy (the mass fraction of the Cu and/or copper-based alloy also comprises alloy formed by excessive Ti in the reaction), and 7-24.3% of TiB2、12.4～43％TiN、0～14.8％BN。
Preferably, the raw materials comprise 15-40% of titanium powder, 5-20% of boron nitride powder and 80-30% of copper powder or/and copper-based alloy powder by mass based on 100% of the total mass of the raw materials.
Preferably, the alloy element in the copper-based alloy powder may be at least one of lead, tin, aluminum, manganese, titanium, lead, zinc, beryllium, tellurium, antimony, and the like.
Preferably, the average particle size of the titanium powder is 1-50 microns.
Preferably, the average particle size of the boron nitride powder is 0.05-20 microns.
Preferably, the average grain diameter of the copper powder or/and the copper-based alloy powder is 10-100 microns.
Preferably, the atmosphere of the self-propagating sintering is vacuum or inert atmosphere, and is preferably vacuum or Ar gas atmosphere.
In another aspect, the invention also provides a copper-based composite powder prepared according to the method, wherein the phase composition of the copper-based composite powder comprises Cu or/and copper-based alloy, TiB2And TiN.
Preferably, the alloy further comprises a BN phase and/or a Ti phase.
Preferably, the copper-based composite powder comprises 30-80.6% by mass of Cu (and/or copper-based alloy including alloy formed with excessive Ti in reaction) and 7-24.3% by mass of TiB2、12.4～43％TiN、0～14.8％BN。
The copper-based composite powder prepared by the invention can be applied to preparing enhanced self-lubricating copper-based composite materials so as to improve the mechanical and wear-resisting properties of the materials, and is applied to the fields of brake pads, worm gears, motor brushes and the like. The copper-based composite powder prepared by the invention can also be used as a reinforcement to prepare other metal-based composite materials such as Al, Ti, Mg, Ni and the like.
Compared with the prior art, the copper-based composite powder provided by the invention comprises TiB2the/TiN binary ceramic reinforced phase and the BN lubricating phase can be used for preparing reinforced self-lubricating copper-based composite material and have TiB function2High hardness and high wear resistance of TiN, and high thermal conductivity of pure copper or copper-based alloy. In addition, the introduction of BN lubricating medium is beneficial to obtaining lower and more stable friction coefficient of the material, reducing the wear rate of the material and meeting the requirements of low wear, long service life and high stability of the copper-based composite material in the application fields of brake pads, gears, worm gears, motor brushes and the like; in addition, the introduction of the ceramic phase can obviously improve the high-temperature mechanical and tribological properties of the material, improve the reliability of the device in a high-temperature environment and have stronger practical value.
Drawings
FIG. 1 is a schematic view of a copper-based composite powder prepared in example 1;
FIG. 2 is an XRD pattern of the copper-based composite powder prepared in example 1;
FIG. 3 is a schematic view of the copper-based composite powder prepared in example 2;
FIG. 4 is an XRD pattern of the copper-based composite powder prepared in example 2;
FIG. 5 is a schematic view of the copper-based composite powder prepared in example 3;
fig. 6 is an XRD pattern of the copper-based composite powder prepared in example 3.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
The copper-based composite powder is prepared by taking pure titanium powder, boron nitride powder and copper or/and copper-based alloy powder as raw materials, uniformly mixing (ball milling and the like can be adopted in a mixing mode) and then carrying out self-propagating sintering.
Preferably, the raw material consists of titanium powder, boron nitride powder, copper or copper-based alloy powder.
The following examples illustrate the preparation method of the copper-based composite powder provided by the present invention.
The raw materials comprise 15-50% by mass of titanium powder, 5-20% by mass of boron nitride powder and 80-40% by mass of copper powder.
In a further preferable scheme, the mass fraction of the titanium powder is 15-40%, the mass fraction of the boron nitride powder is 5-20%, and the mass fraction of the copper powder is 80-40%.
The raw materials are weighed according to the proportion and then evenly mixed to obtain raw material powder. The manner of uniform mixing includes, but is not limited to, milling, ball milling, etc. And after grinding or ball milling, drying, sieving and the like can be carried out to obtain the raw material powder. Wherein the drying can be ball milling and drying at 50-80 ℃ for 2-6 hours. The sieve can be generally 100 meshes. The average particle size of the titanium powder in the raw material powder can be 1-50 μm. The average particle size of the boron nitride powder can be 0.05-20 μm. The average particle diameter of the copper or copper-based alloy powder may be 10 to 100 μm. On the basis of ensuring that Ti powder and BN powder fully react in the self-propagating process, the wider powder particle size range is beneficial to reducing the difficulty of material selection and reducing the production cost.
And carrying out self-propagating sintering on the obtained raw material powder to obtain the copper-based composite powder. Specifically, the mixture powder is placed in a graphite crucible and is sintered in a self-propagating sintering furnace to obtain the required copper-based composite powder. The atmosphere adopted by the self-propagating sintering process is vacuum or inert atmosphere, such as Ar gas or other inert atmosphere. In the self-propagating sintering process, the temperature is achieved spontaneously through reaction, and no specific temperature requirement exists.
As an example of a method for preparing a copper-based composite powder, there is included:
a) weighing titanium powder, boron nitride powder and copper or copper-based alloy powder according to the proportion;
b) ball milling to uniformly mix the powder to prepare raw material powder;
b) and (4) carrying out self-propagating sintering on the raw material powder obtained in the previous step to obtain the required composite powder.
The invention also provides a reinforced self-lubricating copper-based composite material prepared from the copper-based composite powder. Specifically, the obtained copper-based composite powder is molded and sintered to obtain the enhanced self-lubricating copper-based composite material. The forming method includes, but is not limited to, dry pressing, hot pressing, cold isostatic pressing, etc.
The main component of the copper-based composite powder prepared by the invention is TiB2TiN, Cu or/and Cu-based alloys, and may further include a BN phase and/or a Ti phase. Prepared by the invention and containing TiB2The copper-based composite powder of TiN, Cu-based alloy, BN, Ti and other components can be used for preparing enhanced self-lubricating copper-based composite material, wherein TiB2The material can meet the application requirements of brake pads, gears, worm gears or motor brushes and the like by taking the/TiN as a binary enhanced phase and the BN as a self-lubricating medium; in addition, the composite powder can also be used as a reinforcing phase to prepare other metal matrix composite materials such as Al, Ti, Mg, Ni and the like.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Firstly, weighing 5g of boron nitride powder with a median particle size of 0.5 mu m, 14.4g of pure titanium powder with a median particle size of 40 mu m and 14g of pure copper powder with a median particle size of 40 mu m, adding 40g of absolute ethyl alcohol, and performing rolling ball milling for 3 hours to prepare uniform and stable slurry; then drying for 2 hours at 50-80 ℃, and sieving to obtain mixture powder; and placing the mixture powder into a graphite crucible, and placing the graphite crucible into a self-propagating sintering furnace for sintering to obtain the required copper-based composite powder.
The powder morphology of the copper-based composite powder prepared in this example is shown in fig. 1, and the phase composition is shown in fig. 2. As can be seen from FIG. 1, the particle size of the composite powder was in the range of 10 to 50 μm, and it was judged that the reinforcing phase ceramic particles were adhered to the copper particles to form a structure. From FIG. 2, it can be seen that the phase composition of the composite powder includes TiB2TiN, Cu and BN, and in this example, it can be seen that the presence of a BN phase was not detected in the product, and that the reaction of BN was complete.
Example 2
Firstly, weighing 6g of boron nitride powder with the median particle size of 0.5 mu m, 15g of pure titanium powder with the median particle size of 40 mu m and 9g of pure copper powder with the median particle size of 40 mu m, adding 40g of absolute ethyl alcohol, and performing rolling ball milling for 3 hours to prepare uniform and stable slurry; then drying for 2 hours at 50-80 ℃, and sieving to obtain mixture powder; and placing the mixture powder into a graphite crucible, and placing the graphite crucible into a self-propagating sintering furnace for sintering to obtain the required copper-based composite powder.
The powder morphology of the copper-based composite powder prepared in this example is shown in fig. 3, and the phase composition is shown in fig. 4. As can be seen from fig. 3, the fine particles adhered to the surface of the product particles and the particle size was in the submicron level, and it was judged that the adhered matter was excess unreacted BN particles. From FIG. 4, it can be seen that the phase composition of the composite powder includes TiB2TiN, Cu and BN.
Example 3
Firstly, weighing 7.5g of boron nitride powder with the median particle size of 0.5 mu m, 14.4g of pure titanium powder with the median particle size of 40 mu m and 9.4g of pure copper powder with the median particle size of 40 mu m, adding 40g of absolute ethyl alcohol, and performing rolling ball milling for 3 hours to prepare uniform and stable slurry; then drying for 2 hours at 50-80 ℃, and sieving to obtain mixture powder; and placing the mixture powder into a graphite crucible, and placing the graphite crucible into a self-propagating sintering furnace for sintering to obtain the required copper-based composite powder.
The powder morphology of the copper-based composite powder prepared in this example is shown in fig. 5, and it can be seen from the figure that the surfaces of the composite powder particles are covered by a large amount of submicron fine particles, and the particle size indicates that the submicron particles are BN. The phase composition is shown in FIG. 6, from which it can be seen that the phase composition of the composite powder comprises TiB2TiN, Cu and BN.
Example 4
Firstly, weighing 5g of boron nitride powder with a median particle size of 0.5 mu m, 19.4g of pure titanium powder with a median particle size of 40 mu m and 14.4g of pure copper powder with a median particle size of 40 mu m, adding 40g of absolute ethyl alcohol, and performing rolling ball milling for 3 hours to prepare uniform and stable slurry; then drying for 2 hours at 50-80 ℃, and sieving to obtain mixture powder; and placing the mixture powder into a graphite crucible, and placing the graphite crucible into a self-propagating sintering furnace for sintering to obtain the required copper-based composite powder.
Example 5
Firstly, 5g of boron nitride powder with the median particle size of 0.5 mu m, 15g of pure titanium powder with the median particle size of 40 mu m and 80g of copper-tin alloy powder with the median particle size of 40 mu m (the trade mark is QSN5, the national standard of corresponding components can be found according to the trade mark) are weighed, 40g of absolute ethyl alcohol is added, and the mixture is rolled and ball-milled for 3 hours to prepare uniform and stable slurry; then drying for 2 hours at 50-80 ℃, and sieving to obtain mixture powder; and placing the mixture powder into a graphite crucible, and placing the graphite crucible into a self-propagating sintering furnace for sintering to obtain the required copper-based composite powder.
Table 1 shows the components and contents of the composite powder prepared in each example:
Claims (2)
1. a process for synthesizing copper-base composite powder by self-spreading method includes such steps as mixing Ti powder, B nitride powder and Cu powder to obtain mixture powder, putting the mixture powder in graphite crucible, and self-spreading sintering to obtain TiB2TiN, Cu and BN, and submicron BN particles are attached to the surface of the copper-based composite powder; the atmosphere of the self-propagating sintering is vacuum or inert atmosphere;
the mass fraction of titanium powder in the raw material is 40-50%, the mass fraction of boron nitride powder is 5-20%, and the mass fraction of copper powder is 40-30% based on 100% of the total mass of the raw material;
the average particle size of the titanium powder is 40-50 microns, the average particle size of the boron nitride powder is 0.05-0.5 microns, and the average particle size of the copper powder is 40-100 microns, so that the Ti powder and the BN powder can be fully reacted in the self-propagating process.
2. The method according to claim 1, wherein the atmosphere of the self-propagating sintering is an Ar gas atmosphere.
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