CN110695362A - Fe-Cr-based composite ceramic material and preparation method thereof - Google Patents
Fe-Cr-based composite ceramic material and preparation method thereof Download PDFInfo
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- 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
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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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
Abstract
The invention belongs to the field of ceramic materials, and particularly relates to a Fe-Cr-based composite ceramic material and a preparation method thereof. The Fe-Cr based composite ceramic material consists of Fe powder and Cr2O3Powder, Al2O3Powder composition according to the qualityThe content of Fe powder is 45 ~ 50% and Cr is calculated by weight percentage2O335 ~ 40% of powder, Al2O3The powder content is 10 ~ 20%, and the preparation method of the Fe-Cr-based composite ceramic material comprises the steps of material preparation, ball milling, additive stirring, gel forming, kerosene soaking, degreasing, high-temperature sintering, vibration milling and machining.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to a Fe-Cr-based composite ceramic material and a preparation method thereof.
Background
Under the working environment of high temperature, high humidity and strong corrosion, metal components are very easy to lose efficacy and scrap due to the severe service environment, and the service life is severely limited, while ceramic materials are widely applied to the fields of electronics, chemical industry, machinery, metallurgy and the like due to a series of excellent physicochemical properties such as high hardness, wear resistance, good chemical stability, low price and the like. However, the traditional single-phase ceramic materials, such as high-alumina ceramic and zirconia ceramic, have low toughness and high brittleness, which limits the application in engineering, and meanwhile, the ceramic materials are not easy to be cold-processed, not easy to be processed into complex geometric structures, or the processing cost is very expensive, thereby limiting the popularization of the single-phase ceramic materials. In order to solve the problem of low fracture toughness of single-phase ceramics, composite ceramic materials are gradually developed, and various intermetallic compounds are adopted to toughen the single-phase ceramics, so that the toughness of the single-phase ceramics can be effectively improved. The performance of the composite ceramic material is closely related to the type and collocation of the composite phase and the particle size of powder, and is also closely related to a plurality of preparation processes such as ball milling, powder dispersion degree, sintering and the like, so that the composite ceramic which is developed and has high temperature resistance, corrosion resistance, high strength, high toughness and good cutting processing performance has higher engineering difficulty.
Disclosure of Invention
Based on the background, the invention provides the Fe-Cr-based composite ceramic material and the preparation method thereof, and the prepared Fe-Cr-based composite ceramic material has the advantages of high temperature resistance, corrosion resistance, low expansion coefficient, high strength, high toughness, good machining performance and the like.
The invention provides a Fe-Cr based composite ceramic material, which comprises the components of Fe powder and Cr2O3Powder, Al2O3Powder, preferably, the content of the Fe powder is 45 ~ 50% by mass percent, and the Cr is2O3The powder content is 35 ~ 40%, and the Al content is2O3The powder content was 10 ~ 20%.
Preferably, the purity of the Fe powder is more than or equal to 99.9 percent, the particle size of the Fe powder is 60-200nm, and the Cr is2O3The purity of the powder is more than or equal to 99.9 percent, and the Cr is2O3The particle size of the powder is 50-500nm, and the Al is2O3Purity of the powder is greater than or equal to 95%, and the Al2O3The particle size of the powder is 50-500 nm.
The invention also provides a preparation method of the Fe-Cr-based composite ceramic material, which comprises the following steps:
(1) ball milling: weighing the Fe powder and the Cr according to the proportion2O3Powder and the Al2O3Putting the powder into a ball mill, preferably, the ball mill adopts a polyurethane lining, carrying out wet ball milling for 30 ~ 35h, and then taking out the powder to prepare ball milling slurry, wherein during wet ball milling, the filling rate of a ball milling tank is 70 ~ 80%, deionized water is adopted as a ball milling auxiliary agent, and the addition amounts of Fe powder and Cr powder are 70% and ~%, respectively2O3Powder and Al2O30.8 percent of the total mass of the powder, and the ball milling medium is agate balls, the particle size of the agate balls is 20 ~ 25mm, the ball-material ratio is 2, and the ball milling rotating speed is 30 ~ 35 r/min.
(2) Pulping, namely adding methyl cellulose into the ball-milling slurry prepared in the step (1) and then starting stirring, preferably, adding the methyl cellulose in an amount which is 10 ~ 15% of the mass of the ball-milling slurry, adding a suspending agent and a gelling agent simultaneously while stirring, preferably, adding the suspending agent and the gelling agent in amounts which are 3 ~ 5% of the mass of the ball-milling slurry,
controlling the stirring speed at 15 ~ 20 rpm and the stirring time at 2 ~ 4h to obtain injection molding slurry;
(3) shaping and degreasing, namely injecting the injection molding dissolving pulp prepared in the step (2) into a mold, standing for 70 ~ 90min, demolding to obtain a blank, placing the blank in a constant temperature chamber at 80 ℃, drying and shaping for 20 ~ 35h, immersing in kerosene for 48h, taking out, placing in a degreasing furnace at 150 ℃, degreasing for 15 ~ 30h, and preparing a degreased blank;
(4) and (4) sintering, namely placing the degreased mixture prepared in the step (3) in a vacuum sintering furnace to sinter for 6 ~ 8 hours at the sintering temperature of 1430 ~ 1470 ℃, and taking the mixture out of the furnace, and then performing vibration grinding treatment and machining to obtain a finished product of the Fe-Cr-based composite ceramic material.
Compared with the prior art, the invention has the beneficial effects that: the process flow is simple, the cost is low, and the Fe-Cr-based composite ceramic material has the advantages of high temperature resistance, corrosion resistance, low expansion coefficient, high strength, high toughness, good machining performance and the like.
Drawings
FIG. 1 is a flow chart of a method for preparing a Fe-Cr based composite ceramic material.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. The following examples are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of the invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
Weighing 45 percent of Fe powder and 35 percent of Cr according to mass percentage2O3Powder, 20% Al2O3Powder, wherein the purity of Fe powder is 99.9%, the grain diameter is 60nm, and Cr is2O3The purity of the powder was 99.9%, the particle size was 50nm, and Al was added2O3The purity of the powder was 95.0% and the particle size was 50 nm.
Mixing Fe powder and Cr2O3Powder and Al2O3Putting the powder into a ball milling tank with a polyurethane lining, adding agate balls with the particle size of 20mm according to the ball-to-material ratio of 2, and adding Fe powder and Cr2O3Powder and Al2O3Deionized water accounting for 0.8 percent of the total mass of the powder, the loading capacity of a ball milling tank is 75 percent, the ball milling rotating speed is controlled to be 30 r/min, and ball milling is carried out for 30 hours; ball for gameTransferring the ground slurry into a stirring container, adding methylcellulose accounting for 10% of the mass of the ball-milled slurry, setting the stirring speed to be 15 r/min, simultaneously adding a suspending agent and a gelling agent accounting for 3% of the mass of the ball-milled slurry while stirring, and stirring for 2 hours; and injecting the stirred molten slurry into a mold, standing for 70min, demolding, drying and shaping a demolding blank in a constant temperature chamber at 80 ℃ for 20h, immersing in kerosene for 48h, degreasing in a degreasing furnace at 150 ℃ for 15h, transferring the degreased blank into a vacuum sintering furnace, sintering at 1430 ℃ for 8h, taking out, performing vibration grinding treatment, and performing machining to obtain a finished product of the Fe-Cr-based composite ceramic material.
Example 2
Weighing 47% of Fe powder and 38% of Cr according to mass percentage2O3Powder, 15% Al2O3Powder, wherein the purity of Fe powder is 99.9%, the grain diameter is 100nm, and Cr is2O3The purity of the powder is 99.9%, the particle size is 200nm, and Al2O3The purity of the powder was 95.0% and the particle size was 200 nm.
Mixing Fe powder and Cr2O3Powder and Al2O3Putting the powder into a ball milling tank with a polyurethane lining, adding agate balls with the particle size of 22mm according to the ball-to-material ratio of 2, and adding Fe powder and Cr2O3Powder and Al2O3Deionized water accounting for 0.8 percent of the total mass of the powder, the loading capacity of a ball milling tank is 75 percent, the ball milling rotating speed is controlled to be 32 r/min, and ball milling is carried out for 32 hours; transferring the ball-milled slurry into a stirring container, adding methylcellulose accounting for 12% of the mass of the ball-milled slurry, setting the stirring speed to be 18 r/min, simultaneously adding a suspending agent and a gelling agent accounting for 4% of the mass of the ball-milled slurry while stirring, and stirring for 3 hours; and injecting the stirred molten slurry into a mold, standing for 80min, demolding, drying and shaping a demolding blank in a constant temperature chamber at 80 ℃ for 28h, immersing in kerosene for 48h, degreasing in a degreasing furnace at 150 ℃ for 24h, transferring the degreased blank into a vacuum sintering furnace, sintering at 1450 ℃ for 7h, taking out, performing vibration grinding treatment, and performing machining to obtain a finished product of the Fe-Cr-based composite ceramic material.
Example 3
Weighing 50 percent of Fe powder and 40 percent of Cr according to mass percentage2O3Powder, 10% Al2O3Powder, wherein the purity of Fe powder is 99.9%, the grain diameter is 150nm, and Cr2O3The purity of the powder is 99.9%, the particle size is 400nm, and Al2O3The purity of the powder was 95.0% and the particle size was 400 nm.
Mixing Fe powder and Cr2O3Powder and Al2O3Putting the powder into a ball milling tank with a polyurethane lining, adding agate balls with the particle size of 25mm according to the ball-to-material ratio of 2, and adding Fe powder and Cr2O3Powder and Al2O3Deionized water accounting for 0.8 percent of the total mass of the powder, the loading capacity of a ball milling tank is 75 percent, the ball milling rotating speed is controlled to be 35 r/min, and ball milling is carried out for 35 hours; transferring the ball-milled slurry into a stirring container, adding methylcellulose accounting for 15% of the mass of the ball-milled slurry, setting the stirring speed to be 20 r/min, simultaneously adding a suspending agent and a gelling agent accounting for 5% of the mass of the ball-milled slurry while stirring, and stirring for 4 hours; and injecting the stirred molten slurry into a mold, standing for 80min, demolding, drying and shaping a demolding blank in a constant temperature chamber at 80 ℃ for 35h, immersing in kerosene for 48h, degreasing in a degreasing furnace at 150 ℃ for 30h, transferring the degreased blank into a vacuum sintering furnace, sintering at 1470 ℃ for 6h, taking out, carrying out vibration grinding treatment, and then machining to obtain the finished product of the Fe-Cr-based composite ceramic material.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The Fe-Cr based composite ceramic material is characterized by comprising the components of Fe powder and Cr2O3Powder, Al2O3Powder, wherein the content of the Fe powder is 45 ~ 50% by mass, and the Cr is2O3The powder content is 35 ~ 40%, and the Al content is2O3The powder content was 10 ~ 20%.
2. The Fe-Cr based composite ceramic material according to claim 1, whereinCharacterized in that the purity of the Fe powder is more than or equal to 99.9 percent, the granularity of the Fe powder is 60-200nm, and the Cr is2O3The purity of the powder is more than or equal to 99.9 percent, and the Cr is2O3The particle size of the powder is 50-500nm, and the Al is2O3Purity of the powder is greater than or equal to 95.0%, and the Al2O3The particle size of the powder is 50-500 nm.
3. A method for preparing an Fe-Cr based composite ceramic material according to any one of claims 1 to 2, comprising the steps of:
ball milling: weighing the Fe powder and the Cr according to the proportion2O3Powder and the Al2O3Putting the powder into a ball mill, carrying out wet ball milling for 30 ~ 35h, and taking out to obtain ball milling slurry;
pulping, namely adding methyl cellulose into the ball-milled slurry prepared in the step (1), stirring, adding a suspending agent and a gelling agent while stirring, controlling the stirring speed at 15 ~ 20 r/min and the stirring time at 2 ~ 4h, and obtaining injection molding dissolving slurry;
shaping and degreasing, namely injecting the injection molding dissolving pulp prepared in the step (2) into a mold, standing for 70 ~ 90min, demolding to obtain a blank, placing the blank in a constant temperature chamber at 80 ℃, drying and shaping for 20 ~ 35h, immersing in kerosene for 48h, taking out, placing in a degreasing furnace at 150 ℃, degreasing for 15 ~ 30h, and preparing a degreased blank;
and (4) sintering, namely placing the degreased mixture prepared in the step (3) in a vacuum sintering furnace to sinter for 6 ~ 8 hours at the sintering temperature of 1430 ~ 1470 ℃, and taking the mixture out of the furnace, and then performing vibration grinding treatment and machining to obtain a finished product of the Fe-Cr-based composite ceramic material.
4. The preparation method of the Fe-Cr based composite ceramic material as claimed in claim 3, wherein the ball mill in step (1) adopts a polyurethane lining, the filling rate of a ball milling tank is 70 ~ 80% during wet ball milling, deionized water is used as a ball milling aid, and the addition amounts of Fe powder and Cr powder are2O3Powder and Al2O30.8 percent of the total mass of the powder, and agate as a ball milling mediumThe agate balls have the particle size of 20 ~ 25mm, the ball-to-material ratio of 2 and the ball milling rotation speed of 30 ~ 35 revolutions per minute.
5. The method for preparing Fe-Cr based composite ceramic material according to claim 3, wherein the amount of methylcellulose added in step (2) is 10 ~ 15% of the mass of the ball-milled slurry, and the amount of suspending agent and gelling agent are 3 ~ 5% of the mass of the ball-milled slurry.
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| CN1778760A (en) * | 2005-10-18 | 2006-05-31 | 中国海洋大学 | Gel molding-injection base from high-strength ceramic composite materials and shaping method thereof |
| CN101168805A (en) * | 2007-11-09 | 2008-04-30 | 西安交通大学 | Method for preparing ceramic reinforced metal-based porous composite material |
| CN101985399A (en) * | 2009-07-29 | 2011-03-16 | 中国科学院福建物质结构研究所 | Method for preparing Re:YAG polycrystalline transparent ceramics by slip casting and reaction-sintering |
| US20120295113A1 (en) * | 2009-12-28 | 2012-11-22 | Naoki Kurizoe | Method for producing zirconia-alumina composite ceramic material, zirconia-alumina composite granulated powder, and zirconia beads |
| JP2014114201A (en) * | 2012-11-19 | 2014-06-26 | Kyocera Corp | Alumina ceramics and wiring board using the same |
| CN103938006A (en) * | 2013-01-20 | 2014-07-23 | 江苏兆龙电气有限公司 | Manufacturing method of cermet material resistant to molten aluminum corrosion |
| WO2018087224A1 (en) * | 2016-11-09 | 2018-05-17 | Technische Universität Bergakademie Freiberg | Composite material made of metal and ceramic, and method for production thereof |
| US20180369909A1 (en) * | 2015-12-22 | 2018-12-27 | Fujimi Incorporated | Additive manufacturing material for powder lamination manufacturing |
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2019
- 2019-12-03 CN CN201911218510.5A patent/CN110695362B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1778760A (en) * | 2005-10-18 | 2006-05-31 | 中国海洋大学 | Gel molding-injection base from high-strength ceramic composite materials and shaping method thereof |
| CN101168805A (en) * | 2007-11-09 | 2008-04-30 | 西安交通大学 | Method for preparing ceramic reinforced metal-based porous composite material |
| CN101985399A (en) * | 2009-07-29 | 2011-03-16 | 中国科学院福建物质结构研究所 | Method for preparing Re:YAG polycrystalline transparent ceramics by slip casting and reaction-sintering |
| US20120295113A1 (en) * | 2009-12-28 | 2012-11-22 | Naoki Kurizoe | Method for producing zirconia-alumina composite ceramic material, zirconia-alumina composite granulated powder, and zirconia beads |
| JP2014114201A (en) * | 2012-11-19 | 2014-06-26 | Kyocera Corp | Alumina ceramics and wiring board using the same |
| CN103938006A (en) * | 2013-01-20 | 2014-07-23 | 江苏兆龙电气有限公司 | Manufacturing method of cermet material resistant to molten aluminum corrosion |
| US20180369909A1 (en) * | 2015-12-22 | 2018-12-27 | Fujimi Incorporated | Additive manufacturing material for powder lamination manufacturing |
| WO2018087224A1 (en) * | 2016-11-09 | 2018-05-17 | Technische Universität Bergakademie Freiberg | Composite material made of metal and ceramic, and method for production thereof |
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