CN111515404A - Preparation method of cBN/Al composite material - Google Patents
Preparation method of cBN/Al composite material Download PDFInfo
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- CN111515404A CN111515404A CN202010413577.0A CN202010413577A CN111515404A CN 111515404 A CN111515404 A CN 111515404A CN 202010413577 A CN202010413577 A CN 202010413577A CN 111515404 A CN111515404 A CN 111515404A
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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
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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
- 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
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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
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- 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
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- 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
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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
- 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
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- 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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Abstract
The invention relates to a preparation method of a cBN/Al composite material, belonging to the field of aluminum-based composite materials. The preparation method of the cBN/Al composite material comprises the following steps: 1) carrying out high-energy ball milling and mixing on the cBN powder and the Al powder to obtain mixed powder; 2) and pressing the mixed powder into a block, and sintering the block under the protection atmosphere at the temperature of 1000-1300 ℃ without pressure to obtain the powder. The preparation method of the cBN/Al composite material realizes sintering under a non-pressure condition by high-energy ball milling and sintering temperature control, realizes effective combination of the cBN and the Al in the sintering process, and has compact and uniform inner part and no internal defect; 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 the advantages of simple production process, low cost and easy realization of industrial production.
Description
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 aluminum matrix composite material mainly comprises the following reinforcing phases: al (Al)2O3、SiC、Si3N4WC, diamond, etc.
The cubic boron nitride (cBN) has the hardness second to that of diamond, is superior to the diamond in heat conductivity, low thermal expansion coefficient and other excellent performances, can well become the reinforcing phase of the Al-based composite material, has mature production technology and low raw material cost, and has great technical advantages and market advantages when being used as the reinforcing phase of the Al-based composite material.
The existing preparation method of the cBN/Al composite material mainly comprises the methods of hot-pressing sintering, discharge plasma sintering, high-temperature high-pressure sintering and the like, for example, the Chinese patent with the publication number of CN106048278B, namely, the aluminum-based composite material without the generation of a third phase is prepared by adopting the high temperature and the high pressure of 600 ℃ and 4.0 GPa. It can be seen that the existing sintering mode has higher requirements on production equipment, and the hardness is improved to a limited extent, which is not beneficial to large-scale 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 improved to a limited extent.
In order to achieve the purpose, the technical scheme of the preparation method of the cBN/Al composite material is as follows:
a method of making a cBN/Al composite material comprising the steps of:
1) carrying out high-energy ball milling and mixing on the cBN powder and the Al powder to obtain mixed powder;
2) and pressing the mixed powder into a block, and sintering the block under the protection atmosphere at the temperature of 1000-1300 ℃ without pressure to obtain the powder.
The preparation method of the cBN/Al composite material realizes sintering under a non-pressure condition by high-energy ball milling and sintering temperature control, realizes effective combination of the cBN and the Al in the sintering process, and has compact and uniform inner part and no internal defect; 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 the advantages of simple production process, low cost and easy realization of industrial production.
To further optimize the compactness of the product, it is preferable that the cBN powder has a particle size of 3 to 6 μm and the Al powder has a particle size of 0.8 to 1.1 μm.
In order to better improve the hardness and the bonding force of the composite material and promote the reaction of the cBN and the Al to generate the AlN, the volume ratio of the cBN powder to the Al powder is preferably (4-5): (5-6).
In order to promote the pre-combination of the cBN powder and the Al powder and further optimize the compactness of the product, the high-energy ball milling time in the step 1) is preferably at least 0.5 h. The high-energy ball milling is carried out according to the recommended parameters of the high-energy ball milling equipment, for example, the rotating speed of the high-energy ball milling can be controlled to be 1245 RPM.
The block body is pressed in the step 2) only for preparing a pressed blank, the pressed blank has no special requirement on pressing pressure, a single-shaft manual hydraulic press is selected for pressing the block body, and preferably, in the step 2), the pressing pressure is at least 10 MPa.
When the sintering temperature is higher than 1300 ℃, the performance of cBN is greatly weakened, and the pressureless sintering is carried out at the temperature of 1000-1300 ℃, thus having better effect. When pressureless sintering is carried out, the reaction is ensured to be complete, preferably, in the step 2), the pressureless sintering is carried out at the temperature of 1000-1300 ℃ for 1-2 h. In order to further optimize the sintering effect and reduce the sintering stress, preferably, in step 2), before the temperature is raised to 1300 ℃ of 1000-. In order to further improve the uniformity of the sintering process and avoid cracking of the product, the rate of raising the temperature from 300 ℃ at 240 ℃ to 1300 ℃ at 1000 ℃ is preferably 3-5 ℃/min. After sintering, in order to better avoid the generation of stress, avoid the cracking of the product and further optimize the performance of the product, preferably, after pressureless sintering, the product is cooled to room temperature at the speed of not more than 5 ℃/min.
The sintering process has no special requirement on the protective atmosphere, and the protective atmosphere is preferably nitrogen in consideration of the aspects of cost and application effect.
Drawings
FIG. 1 is a graph of the sintering temperature in the method of making a cBN/Al composite of 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 of a cBN/Al composite of example 5 of the invention;
FIG. 4 is the ultrasonic testing results of the cBN/Al composite material of example 5 of the invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings.
In the following examples, cBN (cubic boron nitride) had a particle size of 3 to 6 μm, Al (aluminum) powder had an average particle size of 1 μm, and the particle size distribution ranged mainly from 0.8 μm to 1.1. mu.m.
First, specific example of the method for producing cBN/Al composite material of the invention
Example 1
The preparation method of the cBN/Al composite material 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 carrying out high-energy ball milling for 0.5h (the rotating speed is 1245RPM) to obtain mixed powder;
2) prepressing and molding the mixed powder, keeping the pressing pressure at 10MPa for 30s, placing the molded block in an alumina porcelain boat, conveying the block to the central position of a tubular furnace, sealing two ends of the alumina porcelain boat, introducing nitrogen, and carrying out inert gas protection to avoid the oxidation of the block obtained by molding the pressed composite powder in the sintering process;
setting a temperature rising and reducing program shown in figure 1, heating to 240 ℃ at a temperature rising rate of 5 ℃/min, then preserving heat for 30min, then heating to 1100 ℃ at a temperature rising rate of 5 ℃/min (pressureless sintering), preserving heat for 1h, and then reducing to room temperature at a temperature reducing rate of 5 ℃/min to obtain the cBN/Al composite material.
Example 2
The preparation method of the cBN/Al composite material of the embodiment is different from the embodiment 1 only in that:
in step 1), the volume ratio of the cBN powder to the Al powder was 5: 5.
In the step 2), the temperature of pressureless sintering is 1000 ℃.
Examples 3 to 4
The cBN/Al composite manufacturing methods of examples 3-4 differ from example 2 only in that: in the step 2), the temperature of pressureless sintering is 1100 ℃ and 1300 ℃.
Example 5
The preparation method of the cBN/Al composite material of the embodiment is different from the embodiment 2 only in that: in the step 2), the inert gas is argon; the pressureless sintering temperature was 1300 ℃.
Examples 6 to 7
The cBN/Al composite manufacturing methods of examples 6-7 differ from example 2 only in that: in the step 2), the heat preservation time of the pressureless sintering is 0.5h and 2h respectively (namely, the heat preservation time is 0.5h and 2h respectively after the temperature reaches 1000 ℃).
Second, 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 a hardness tester.
The cBN/Al composite of example 1 has a Vickers hardness of 800 HV.
The hardness values of the cBN/Al composites obtained in examples 2-4 for different sintering temperatures are shown in FIG. 2. As can be seen from FIG. 2, as the sintering temperature increases, the hardness of the cBN/Al composite material increases accordingly, and the Vickers hardness of the sintered article at 1300 ℃ reaches 1050 HV. The resulting cBN/Al composites of examples 6-7 had Vickers hardnesses of 265HV and 318HV, respectively.
The cBN/Al composite of example 5 has a Vickers hardness of 940 HV.
Experimental example 2
XRD analysis was performed on the cBN/Al composite material obtained in example 5, and the results are shown in FIG. 3.
As can be seen from FIG. 3, the reaction of cBN with Al produces AlN, which increases the bonding force and hardness of the cBN/Al composite. 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 information of suitable temperature, sufficient reaction time and sufficient cBN, Al is believed to be converted to AlN.
Experimental example 3
The cBN/Al composite material obtained in example 5 was examined using an ultrasonic flaw detector, and the results are shown in FIG. 4.
As can be seen from FIG. 4, the composite material was dense and uniform in the interior and was free from defects.
In other embodiments of the method of making a cBN/Al composite material of the present invention, the preheating temperature, the holding time, and the heating rate and the cooling rate before reaching the pressureless sintering temperature may be adaptively adjusted within the ranges defined in the present invention, which may all provide superior experimental results comparable to those of the examples.
Claims (10)
1. A preparation method of cBN/Al composite material is characterized by comprising the following steps:
1) carrying out high-energy ball milling and mixing on the cBN powder and the Al powder to obtain mixed powder;
2) and pressing the mixed powder into a block, and sintering the block under the protection atmosphere at the temperature of 1000-1300 ℃ without pressure to obtain the powder.
2. The method of manufacturing a cBN/Al composite material as claimed in claim 1, wherein the cBN powder has a particle size of 3 to 6 μm and the Al powder has a particle size of 0.8 to 1.1 μm.
3. A method of manufacturing a cBN/Al composite material as claimed in claim 1 or 2, wherein the volume ratio of the cBN powder and the Al powder is (4-5): (5-6).
4. The method of making a cBN/Al composite material as claimed in claim 1, wherein in step 1) the time for the high energy ball milling is at least 0.5 h.
5. A method of making a cBN/Al composite material as claimed in claim 1 characterised in that in step 2) the pressure at which pressing occurs is at least 10 MPa.
6. The method of making a cBN/Al composite material as claimed in claim 1, wherein in step 2) the pressureless sintering is performed at 1000-.
7. The method for preparing a cBN/Al composite material as claimed in claim 6, wherein in step 2), the temperature is first preserved at 300 ℃ for 30-40min before the temperature is raised to 1300 ℃ of 1000-.
8. The method of preparing a cBN/Al composite as claimed in claim 7, wherein the rate of raising the temperature from 240-300 ℃ to 1000-1300 ℃ is 3-5 ℃/min.
9. A method of making a cBN/Al composite material as claimed in any one of claims 1, 6 to 8 characterised in that after pressureless sintering, cooling to room temperature is carried out at a rate of not more than 5 ℃/min.
10. The method of making a cBN/Al composite material as claimed in any one of claims 1, 2, 4-8, characterised in that the protective atmosphere is nitrogen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112267038A (en) * | 2020-09-30 | 2021-01-26 | 哈尔滨工业大学 | Preparation method of BN nanosheet/aluminum-based 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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