CN111515404B - Preparation method of cBN/Al composite material - Google Patents

Preparation method of cBN/Al composite material Download PDF

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Publication number
CN111515404B
CN111515404B CN202010413577.0A CN202010413577A CN111515404B CN 111515404 B CN111515404 B CN 111515404B CN 202010413577 A CN202010413577 A CN 202010413577A CN 111515404 B CN111515404 B CN 111515404B
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cbn
composite material
powder
sintering
preparation
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CN111515404A (en
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江明杰
李和鑫
雷君
王彬彬
黄红卫
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Funik Ultrahard Material Co Ltd
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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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/003—Cubic boron nitrides only

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Products (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to a preparation method of a cBN/Al composite material, and belongs to the field of aluminum-based composite materials. The preparation method of the cBN/Al composite material comprises the following steps: 1) Mixing cBN powder and Al powder by high-energy ball milling to obtain mixed powder; 2) Pressing the mixed powder into a block, and then carrying out pressureless sintering on the block at 1000-1300 ℃ under a protective atmosphere to obtain the composite material. According to the preparation method of the cBN/Al composite material, the sintering under the condition of no pressure is realized through high-energy ball milling and sintering temperature control, the effective combination of the cBN and the Al is realized in the sintering process, and the inside of the cBN/Al composite material is compact and uniform, and has no internal defects; compared with the traditional aluminum alloy material, the hardness and the wear resistance of the cBN/Al composite material are greatly improved; meanwhile, the method has simple production process and low cost, and is easy to realize industrialized production.

Description

Preparation method of cBN/Al composite material
Technical Field
The invention belongs to the field of aluminum-based composite materials, and particularly relates to a preparation method of a cBN/Al composite material.
Background
The aluminum-based composite material has the advantages of small density, good thermal stability, electric conduction, strong designability and the like, and is widely applied to the fields of aerospace, automobiles, sports goods and the like. At present, the current time of the process,the reinforcing phases used in the aluminum matrix composite material are mainly composed of: al (Al) 2 O 3 、SiC、Si 3 N 4 WC, diamond, etc.
The cubic boron nitride (cBN) has excellent properties of hardness inferior to that of diamond, better than that of diamond, lower thermal expansion coefficient and the like, can be well formed into a reinforcing phase of an Al-based composite material, has mature production technology of the cubic boron nitride micro powder, low raw material cost and has great technical and market advantages as the reinforcing phase of the Al-based composite material.
The existing preparation method of the cBN/Al composite material mainly comprises hot-pressing sintering, spark plasma sintering, high-temperature high-pressure sintering and other methods, for example, the Chinese patent with the publication number CN106048278B adopts high temperature and high pressure of 600 ℃ and 4.0GPa to prepare the aluminum-based composite material without third phase generation. It can be seen that the existing sintering mode has higher requirements on production equipment, and the hardness is limited to be improved, so that the method is not beneficial to mass production.
Disclosure of Invention
The invention aims to provide a preparation method of a cBN/Al composite material, which aims to solve the problems that the production working condition of the existing method is complex and the hardness of the composite material is limited.
In order to achieve the above purpose, the technical scheme of the preparation method of the cBN/Al composite material is as follows:
a preparation method of the cBN/Al composite material comprises the following steps:
1) Mixing cBN powder and Al powder by high-energy ball milling to obtain mixed powder;
2) Pressing the mixed powder into a block, and then carrying out pressureless sintering on the block at 1000-1300 ℃ under a protective atmosphere to obtain the composite material.
According to the preparation method of the cBN/Al composite material, the sintering under the condition of no pressure is realized through high-energy ball milling and sintering temperature control, the effective combination of the cBN and the Al is realized in the sintering process, and the inside of the cBN/Al composite material is compact and uniform, and has no internal defects; compared with the traditional aluminum alloy material, the hardness and the wear resistance of the cBN/Al composite material are greatly improved; meanwhile, the method has simple production process and low cost, and is easy to realize industrialized production.
In order to further optimize the compactibility of the product, it is preferable that the particle size of the cBN powder is 3 to 6. Mu.m, and the particle size of the Al powder is 0.8 to 1.1. Mu.m.
In order to better improve the hardness and the binding force of the composite material and promote the reaction of the cBN and the Al to generate AlN, preferably, the volume ratio of the cBN powder to the Al powder is (4-5): (5-6).
To facilitate pre-bonding of cBN powder and Al powder, further optimizing the density of the article, it is preferred that in step 1) the high energy ball milling time is at least 0.5h. And the high-energy ball milling is performed according to recommended parameters of high-energy ball milling equipment, for example, the rotating speed of the controllable high-energy ball milling is 1245RPM.
The block is pressed in the step 2) only for preparing a pressed compact, no special requirement is imposed on pressing pressure, and a single-shaft manual hydraulic press is selected for pressing the block, preferably, in the step 2), the pressing pressure is at least 10MPa.
When the sintering temperature is higher than 1300 ℃, the performance of the cBN is greatly weakened, and the pressureless sintering is carried out at 1000-1300 ℃, so that the cBN has better effect. The reaction is ensured to be complete during pressureless sintering, and preferably, in the step 2), the pressureless sintering is carried out at 1000-1300 ℃ for 1-2h. In order to further optimize the sintering effect and reduce the sintering stress, it is preferable that in step 2), the temperature is kept at 240-300 ℃ for 30-40min before the temperature is raised to 1000-1300 ℃. In order to further improve the uniformity of the sintering process and avoid cracking of the product, it is preferable that the temperature is raised from 240 to 300 ℃ to 1000 to 1300 ℃ at a rate of 3 to 5 ℃/min. After sintering, to better avoid stress generation, avoid cracking of the product, further optimize product performance, preferably, after pressureless sintering, cooling to room temperature at a rate of no more than 5 ℃/min.
The sintering process has no special requirements on protective atmosphere, and the protective atmosphere is preferably nitrogen from the aspects of cost and application effect.
Drawings
FIG. 1 is a graph showing sintering temperatures in a method for preparing a cBN/Al composite material according to example 1 of the invention;
FIG. 2 is a graph of sintering temperature versus hardness for cBN/Al composites of examples 2-4 of the invention;
FIG. 3 is an XRD pattern for the cBN/Al composite of example 5 of the invention;
FIG. 4 is an ultrasonic flaw detection result of the cBN/Al composite material of example 5 of the invention.
Detailed Description
Embodiments of the present invention will be further described with reference to the accompanying drawings.
In the following examples, the particle size of cBN (cubic boron nitride) was 3 to 6. Mu.m, the average particle size of Al (aluminum) powder was 1. Mu.m, and the particle size distribution was mainly in the range of 0.8 μm to 1.1. Mu.m.
1. Specific examples of the preparation method of the cBN/Al composite material of the invention
Example 1
The preparation method of the cBN/Al composite material of the embodiment adopts the following steps:
1) Weighing cBN powder and Al powder according to a volume ratio of 4:6, adding the cBN powder and the Al powder into a zirconia ball milling tank, selecting zirconia grinding balls, and performing high-energy ball milling for 0.5h (rotating speed 1245 RPM) to obtain mixed powder;
2) Prepressing and forming the mixed powder, wherein the pressing pressure is 10MPa, keeping for 30s, placing the formed block in an alumina porcelain boat, conveying the block to the center of a tube furnace, sealing two ends, and introducing nitrogen for inert gas protection to prevent the block obtained by pressing and forming the composite powder from being oxidized in the sintering process;
setting the temperature rise and fall program shown in figure 1, heating to 240 ℃ at a temperature rise rate of 5 ℃/min, preserving heat for 30min, heating to 1100 ℃ at a temperature rise rate of 5 ℃/min, preserving heat for 1h, and cooling to room temperature at a temperature reduction rate of 5 ℃/min to obtain the cBN/Al composite material.
Example 2
The preparation method of the cBN/Al composite material of this example is different from example 1 only in that:
in step 1), the volume ratio of the cBN powder to the Al powder is 5:5.
In step 2), the pressureless sintering temperature was 1000 ℃.
Examples 3 to 4
The preparation method of the cBN/Al composite material of examples 3 to 4 differs from example 2 only in that: in step 2), the pressureless sintering temperatures were 1100℃and 1300℃respectively.
Example 5
The preparation method of the cBN/Al composite material of this example is different from example 2 only in that: in the step 2), the inert gas is argon; the pressureless sintering temperature was 1300 ℃.
Examples 6 to 7
The preparation method of the cBN/Al composite material of examples 6 to 7 differs from example 2 only in that: in step 2), the pressureless sintering is carried out for 0.5h and 2h respectively (i.e. after reaching 1000 ℃ for 0.5h and 2h respectively).
2. Experimental example
Experimental example 1
The cBN/Al composite materials obtained in examples 1 to 5 were subjected to a flat grinding and polishing treatment and then tested for Vickers hardness by using a durometer.
The cBN/Al composite of example 1 has a Vickers hardness of 800HV.
The cBN/Al composites obtained in examples 2-4 have hardness values corresponding to different sintering temperatures as shown in FIG. 2. As can be seen from fig. 2, as the sintering temperature increases, the hardness of the cBN/Al composite increases accordingly, and the vickers hardness of the sintered product at 1300 ℃ reaches 1050HV. The cBN/Al composites obtained in examples 6-7 had Vickers hardness of 265HV and 318HV, respectively.
The cBN/Al composite of example 5 has a Vickers hardness of 940HV.
Experimental example 2
XRD analysis was performed on the cBN/Al composite material obtained in example 5, and the result is shown in FIG. 3.
As can be seen from fig. 3, cBN reacts with Al to form AlN, thereby increasing the bonding force and hardness of the cBN/Al composite material. The absence of Al phase in the XRD pattern demonstrates that the Al content in the composite is less than 5%, and in addition, in combination with the proper temperature, sufficient reaction time, and sufficient cBN information, it is believed that Al is converted to AlN.
Experimental example 3
The cBN/Al composite material obtained in example 5 was examined by using an ultrasonic flaw detector, and the results are shown in FIG. 4.
As can be seen from fig. 4, the composite material was internally densified and uniform, and had no defects.
In other embodiments of the method for preparing a cBN/Al composite material of the present invention, the preheating temperature, the holding time, the heating rate, and the cooling rate before reaching the pressureless sintering temperature may be adaptively adjusted within the range defined by the present invention, which may all achieve superior experimental effects comparable to those of the embodiments.

Claims (8)

1. The preparation method of the cBN/Al composite material is characterized by comprising the following steps of:
1) Mixing cBN powder and Al powder by high-energy ball milling to obtain mixed powder;
2) Pressing the mixed powder into blocks, then carrying out pressureless sintering on the blocks at 1000-1300 ℃ under protective atmosphere to obtain the composite material,
the particle size of the cBN powder is 3-6 mu m, the particle size of the Al powder is 0.8-1.1 mu m, and the volume ratio of the cBN powder to the Al powder is (4-5): (5-6).
2. The method of producing cBN/Al composite material as claimed in claim 1, wherein in the step 1), the time of the high energy ball milling is at least 0.5h.
3. A method of producing a cBN/Al composite material as claimed in claim 1, wherein in step 2), the pressure at the time of pressing is at least 10MPa.
4. The method of producing cBN/Al composite material as claimed in claim 1, wherein in the step 2), the pressureless sintering is performed at 1000 to 1300 ℃ for 1 to 2 hours.
5. The method of producing cBN/Al composite material as claimed in claim 4, wherein in step 2), heat is preserved for 30 to 40 minutes at 240 to 300 ℃ before heating to 1000 to 1300 ℃.
6. A method of producing a cBN/Al composite material as claimed in claim 5, wherein the rate of temperature rise from 240 to 300 ℃ to 1000 to 1300 ℃ is 3 to 5 ℃/min.
7. A method of producing a cBN/Al composite material as claimed in any one of claims 1, 4 to 6, wherein after pressureless sintering, cooling to room temperature is performed at a rate of not more than 5 ℃/min.
8. A method of producing a cBN/Al composite material as claimed in any one of claims 1 to 6, wherein the protective atmosphere is nitrogen.
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CN112267038B (en) * 2020-09-30 2022-03-04 哈尔滨工业大学 Preparation method of BN nanosheet/1060 Al composite material
CN112661517A (en) * 2020-12-31 2021-04-16 富耐克超硬材料股份有限公司 Preparation method of heat dissipation composite material

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