CN100448798C - Method for preparing carborundum whisker reinforced carborundum composite material element - Google Patents
Method for preparing carborundum whisker reinforced carborundum composite material element Download PDFInfo
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- CN100448798C CN100448798C CNB2007100989038A CN200710098903A CN100448798C CN 100448798 C CN100448798 C CN 100448798C CN B2007100989038 A CNB2007100989038 A CN B2007100989038A CN 200710098903 A CN200710098903 A CN 200710098903A CN 100448798 C CN100448798 C CN 100448798C
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Abstract
A producing method for enhanced silicon carbide compound material parts by the silicon carbide whisker belongs to the preparation techical field of ceramic substrate compound material and parts thereof. The SiCw/SiC compound material parts are produced by a combined art of powder injecting molding and precursor transformation. An even feed is obtained by mixing the SiC micro powder and SiC whisker and prepared binder in a certain proportion. The feed is injecting molding in the injecting molding machine by die after pelletization and obtaining a molding base of SiCw/SiC compound material part with needed shape. The molding base of SiCw/SiC compound material part is pre-sintered in 1300-1500 DEG C after thermally degreasing, finally sintered to densification in the sintering kiln. The advantages of the invention is: reducing the application amount of the powder injecting molding SiC ceramic binder, increasing the parts capacity and size accuracy and production efficiency, achieving the complicated SiCw/SiC compound material parts of near-final, low cost and mass production.
Description
Technical field
The invention belongs to the preparing technical field of ceramic matric composite and component thereof, a kind of method of preparation nearly end form carborundum whisker reinforced carborundum (SiCw/SiC) composite material parts particularly is provided, has realized preparation low-cost, the high performance ceramic base composite material parts.
Background technology
Developing rapidly of modern national defense, nuclear energy and aeronautical and space technology and petrochemical complex, oceanographic engineering etc., numerous critical materials such as rocket chamber liner, aircraft turbine engine blades, nuclear reactor structure parts, high speed pneumatic bearing, mechanical seal part, lightweight satellite reflection mirror are proposed more and more high requirement, pressed for the various novel high performance materials of exploitation.Silicon carbide (SiC), silicon nitride (Si
3N
4) wait advanced ceramics to have the hot strength height because of it, advantage such as resistance to abrasion, oxidation-resistance, anti-thermal shock and Heat stability is good and thermal expansivity are little, density is low is used widely in a lot of fields.The inherent fragility of pottery own makes it be difficult to accomplish something in the high-temperature material field always, therefore, and the toughness reinforcing research topic that become international of advanced ceramics.In all method for toughening, ceramic fiber and crystal whisker excess weld metal toughening ceramic based composites are shown up prominently in structure applications in the great potential aspect high strength and the high tenacity because of it.Wherein, the SiC whisker (SiCw) with diamond-type structure becomes one of of paramount importance strengthening and toughening agent in the ceramic matric composite.
Because SiCw/SiC matrix material not only matrix itself has excellent high-temperature behavior, SiCw is compatible fully with the SiC matrix simultaneously, whisker can be brought into play the strengthening and toughening effect well, so the SiCw/SiC matrix material is considered to following one of internal combustion turbine, rocket nozzle, engine and most promising candidate materials in field such as heat exchanger component and satellite reflection mirror made.
The manufacturing process of SiCw enhancing SiC matrix material mainly contains traditional powder metallurgy and is molded into shape, precursor infiltration and pyrolysis method, casting and press filtration shaping etc.Though traditional powder metallurgy compression molding technology is simple, the shaping base that mold pressing forms often density unevenness is even, and the complex-shaped degree of parts also is subjected to certain restriction.And also there are shortcomings such as preparation cycle is long, dimensional precision is low in the precursor infiltration and pyrolysis method except that being subjected to the restriction of parts complexity.The complicated form part that can be shaped though casting and press filtration are shaped is owing to problems such as shaping base density uniformity difference and dimensional precision are low have limited its range of application.Therefore, can directly prepare have net shape, the component of dimensional precision height and excellent performance, be that SiCw strengthens the key that ceramic matric composite can be used widely.
The present invention adopts powder injection forming to transform combine prepared SiCw/SiC matrix material and part thereof with precursor.Powder injection forming is the novel nearly end form forming technique that modern plastics injection molding technology introducing field of powder metallurgy is formed.The maximum characteristics of this technology are directly to prepare complex-shaped, homogeneous microstructure, nearly end form part that dimensional precision is high, have plurality of advantages such as cost is low, efficient is high, application is wide.
In order further to improve the performance and the production efficiency of SiCw/SiC composite material parts, the present invention introduces the precursor conversion process and prepares the SiCw/SiC composite material parts on the powder injection forming basis.Studies show that, add the densification temperature that a certain amount of SiC precursor (Polycarbosilane) can significantly reduce the SiC pottery in the SiC matrix powder, this is because the fine SiC crystal that is transformed by Polycarbosilane in SiC ceramic densifying process helps the densification of SiC pottery.In addition, Polycarbosilane inherent organic trait makes it be well suited for binding agent as powder injection forming SiC pottery.Therefore, adopt Polycarbosilane not only can reduce the densification temperature of injection forming SiC pottery as the injecting forming binder major ingredient, improve the performance of part, the usage quantity of other binding agent when also greatly having reduced powder injection forming SiC pottery simultaneously, thus the degreasing efficient of part forming base and the dimensional precision of part improved.Therefore, adopt powder injection forming to transform the shaping problem that the prepared SiCw/SiC composite material parts that combines can thoroughly solve the SiCw/SiC composite material parts, realize low cost, the mass production of SiCw/SiC composite material parts with precursor.
Summary of the invention
The object of the present invention is to provide a kind of method of the SiCw/SiC of preparation composite material parts, solved the shaping problem of SiCw/SiC composite material parts, can realize the preparation of low cost, high-performance SiCw/SiC composite material parts.
The present invention adopts powder injection forming to transform the prepared SiCw/SiC composite material parts that combines with precursor.Adopt the precursor conversion process not only can reduce the densification temperature of injection forming SiC pottery, improve the performance of part, go back the usage quantity of other binding agent when significantly reducing powder injection forming SiC pottery simultaneously, thereby improved the degreasing efficient and the parts size precision of shaping base.Concrete technology is:
At first selected SiC micro mist and SiC whisker were being become uniform feeding with the binding agent of being prepared on the mixing roll after under 120 ℃～140 ℃ temperature mixing 1.5～2 hours, the powder loading capacity is 54～60 volume %.Feeding after granulating on the injection machine under 140～160 ℃ of temperature, 100～120MPa pressure injection forming, obtain the SiCw/SiC composite material parts shaping base of desired shape.The SiCw/SiC composite material parts shaping base of gained after overheated degreasing, presintering under 1300～1500 ℃ of temperature.At last the SiCw/SiC composite material parts is placed sintering oven under 1850～1950 ℃ of temperature, argon gas atmosphere protection, to carry out sintering, obtain qualified SiCw/SiC composite material parts.Technical process as shown in Figure 1.
The binding agent that the present invention prepared is Polycarbosilane base (PCS) multicomponent binding agent, with paraffin wax (PW) and high density polyethylene(HDPE) (HDPE) as softening agent, with stearic acid (SA) is tensio-active agent, and each constituent element weight percent is PCS: PW: HDPE: SA=(40～60): (30～45): (5～10): (0～5).
The mass ratio of SiC micro mist and SiC whisker is 100 in the feeding: (8～25)
The feeding back of granulating is shaped on injection machine, and forming temperature is that 140～160 ℃, pressure are 100～120MPa on injection machine, and pre-sintering temperature is 1300～1500 ℃.
Precursor transforms and shaping base pre-sintering process is: continue to be warming up to 900 ℃～1100 insulations after 0.5 hour through the shaping base after the hot degreasing, be warming up to 1300～1500 ℃ and be incubated 1 hour then.
Because SiC powder and Polycarbosilane Quito constituent element binding agent are mixed into uniform feeding, feeding after granulating on injection machine injection forming obtain SiCw/SiC composite material parts shaping base, therefore, shaping base density is even, does not need any mechanical process.Feeding can reuse simultaneously, and material use efficiency reaches 100%.SiCw/SiC composite material parts shaping base obtains the dimensional precision height behind degreasing, presintering and final sintering, without any need for the SiCw/SiC composite material parts of aftertreatment, products obtained therefrom is not only organized with performance even, the size of product and consistency of performance might as well, and can be mass-produced, cost is low.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
With SiC micro mist and SiC whisker SiC micro mist by mass percentage: the mixed of SiC whisker=100: 8 evenly makes premixed powder.Binding agent adopts Polycarbosilane Quito constituent element binding agent, and its each constituent element weight percent is PCS: PW: HDPE: SA=40: 45: 10: 5.With this binding agent on the mixing roll in after under 120 ℃ of temperature mixing 2 hours with premixed powder on the mixing roll under 120 ℃ of temperature mixing 2 hours, the powder loading capacity is 54 volume %.Granulation back injection forming on injector, injection temperature is 140 ℃, and injection pressure is 110MPa, and the mould temperature is 30 ℃.Gained SiCw/SiC composite material parts shaping base is warming up to 200 ℃ of insulations 0.5 hour in the thermal debinding furnace under the hydrogen shield, is warming up to 380 ℃ of insulations 0.5 hour again, continue to be warmed up to 500 ℃ and be incubated 1 hour to remove binding agent fully.Part forming base after the degreasing is continued to be warming up to 900 ℃ of insulations after 0.5 hour, be warming up to 1300 ℃ and be incubated 1 hour again, thereby finish the conversion of precursor and the presintering of shaping base, obtain SiCw/SiC composite material parts presintered compact.At last presintered compact is placed sintering oven to protect following sintering 2 hours, promptly get SiCw/SiC composite material parts product in 1850 ℃ of temperature, argon gas atmosphere.
Embodiment 2:
With SiC micro mist and SiC whisker SiC micro mist by mass percentage: the mixed of SiC whisker=100: 15 evenly makes premixed powder.Binding agent adopts Polycarbosilane Quito constituent element binding agent, and its each constituent element weight percent is PCS: PW: HDPE: SA=50: 40: 5: 5.With this binding agent on the mixing roll in after under 130 ℃ of temperature mixing 1.5 hours with premixed powder on the mixing roll under 120 ℃ of temperature mixing 2 hours, the powder loading capacity is 58 volume %.Granulation back injection forming on injector, injection temperature is 150 ℃, and injection pressure is 100MPa, and the mould temperature is 30 ℃.Gained SiCw/SiC composite material parts shaping base is warming up to 200 ℃ of insulations 0.5 hour in the thermal debinding furnace under the hydrogen shield, is warming up to 380 ℃ of insulations 0.5 hour again, continue to be warmed up to 500 ℃ and be incubated 1 hour to remove binding agent fully.Part forming base after the degreasing is continued to be warming up to 900 ℃ of insulations after 0.5 hour, be warming up to 1400 ℃ and be incubated 1 hour again, thereby finish the conversion of precursor and the presintering of shaping base, obtain SiCw/SiC composite material parts presintered compact.At last presintered compact is placed sintering oven to protect following sintering 2 hours, promptly get SiCw/SiC composite material parts product in 1850 ℃ of temperature, argon gas atmosphere.
Embodiment 3:
With SiC micro mist and SiC whisker SiC micro mist by mass percentage: the mixed of SiC whisker=100: 15 evenly makes premixed powder.Binding agent adopts Polycarbosilane Quito constituent element binding agent, and its each constituent element weight percent is PCS: PW: HDPE: SA=60: 30: 10: 0.With this binding agent on the mixing roll in after under 130 ℃ of temperature mixing 1.5 hours with premixed powder on the mixing roll under 130 ℃ of temperature mixing 2 hours, the powder loading capacity is 58 volume %.Granulation back injection forming on injector, injection temperature is 150 ℃, and injection pressure is 110MPa, and the mould temperature is 30 ℃.Gained SiCw/SiC composite material parts shaping base is warming up to 200 ℃ of insulations 0.5 hour in the thermal debinding furnace under the hydrogen shield, is warming up to 420 ℃ of insulations 0.5 hour again, continue to be warmed up to 520 ℃ and be incubated 1 hour to remove binding agent fully.Part forming base after the degreasing is continued to be warming up to 1000 ℃ of insulations after 0.5 hour, be warming up to 1500 ℃ and be incubated 1 hour again, thereby finish the conversion of precursor and the presintering of shaping base, obtain SiCw/SiC composite material parts presintered compact.At last presintered compact is placed sintering oven to protect following sintering 2 hours, promptly get SiCw/SiC composite material parts product in 1900 ℃ of temperature, argon gas atmosphere.
Embodiment 4:
With SiC micro mist and SiC whisker SiC micro mist by mass percentage: the mixed of SiC whisker=100: 20 evenly makes premixed powder.Binding agent adopts Polycarbosilane Quito constituent element binding agent, and its each constituent element weight percent is PCS: PW: HDPE: SA=50: 40: 7: 3.With this binding agent on the mixing roll in after under 140 ℃ of temperature mixing 1.5 hours with premixed powder on the mixing roll under 140 ℃ of temperature mixing 1.5 hours, the powder loading capacity is 60 volume %.Granulation back injection forming on injector, injection temperature is 160 ℃, and injection pressure is 120MPa, and the mould temperature is 30 ℃.Gained SiCw/SiC composite material parts shaping base is warming up to 200 ℃ of insulations 0.5 hour in the thermal debinding furnace under the hydrogen shield, is warming up to 400 ℃ of insulations 0.5 hour again, continue to be warmed up to 540 ℃ and be incubated 1 hour to remove binding agent fully.Part forming base after the degreasing is continued to be warming up to 1100 ℃ of insulations after 0.5 hour, be warming up to 1500 ℃ and be incubated 1 hour again, thereby finish the conversion of precursor and the presintering of shaping base, obtain SiCw/SiC composite material parts presintered compact.At last presintered compact is placed sintering oven to protect following sintering 2 hours, promptly get SiCw/SiC composite material parts product in 1950 ℃ of temperature, argon gas atmosphere.
Embodiment 5:
With SiC micro mist and SiC whisker SiC micro mist by mass percentage: the mixed of SiC whisker=100: 15 evenly makes premixed powder.Binding agent adopts Polycarbosilane Quito constituent element binding agent, and its each constituent element weight percent is PCS: PW: HDPE: SA=60: 30: 10: 0.With this binding agent on the mixing roll in after under 130 ℃ of temperature mixing 1.5 hours with premixed powder on the mixing roll under 130 ℃ of temperature mixing 1.5 hours, the powder loading capacity is 58 volume %.Granulation back injection forming on injector, injection temperature is 160 ℃, and injection pressure is 100MPa, and the mould temperature is 30 ℃.Gained SiCw/SiC composite material parts shaping base is warming up to 200 ℃ of insulations 0.5 hour in the thermal debinding furnace under the hydrogen shield, is warming up to 420 ℃ of insulations 0.5 hour again, continue to be warmed up to 520 ℃ and be incubated 1 hour to remove binding agent fully.Part forming base after the degreasing is continued to be warming up to 1000 ℃ of insulations after 0.5 hour, be warming up to 1500 ℃ and be incubated 1 hour again, thereby finish the conversion of precursor and the presintering of shaping base, obtain SiCw/SiC composite material parts presintered compact.At last presintered compact is placed sintering oven to protect following sintering 2 hours, promptly get SiCw/SiC composite material parts product in 1950 ℃ of temperature, argon gas atmosphere.
Claims (1)
1, a kind of method for preparing carborundum whisker reinforced carborundum composite material element is characterized in that: adopt powder injection forming to transform the prepared SiCw/SiC composite material parts that combines with precursor; Technology is: selected SiC micro mist and SiC whisker were being become uniform feeding with the binding agent of being prepared on the mixing roll after under 120 ℃～140 ℃ temperature mixing 1.5～2 hours, the powder loading capacity is 54～60 volume %, feeding after granulating on the injection machine under 140～160 ℃ of temperature, 100～120MPa pressure injection forming, obtain the SiCw/SiC composite material parts shaping base of desired shape; The SiCw/SiC composite material parts shaping base of gained after overheated degreasing, presintering under 1300～1500 ℃ of temperature; At last SiCw/SiC composite material parts presintered compact is placed sintering oven under 1850～1950 ℃ of temperature, argon gas atmosphere protection, to carry out sintering, obtain qualified SiCw/SiC composite material parts;
The binding agent of being prepared is the Polycarbosilane based binder, with paraffin wax and high density polyethylene(HDPE) as softening agent, with the stearic acid is tensio-active agent, and each constituent element weight percent is the Polycarbosilane base: paraffin wax: high density polyethylene(HDPE): stearic acid=(40～60): (30～45): (5～10): (0～5);
The weight ratio of SiC micro mist and SiC whisker is 100 in the feeding: (8～25);
The hot degreasing process of shaping base is: at first be warming up to 200 ℃ of insulations 0.5 hour, and then be warming up to 380～420 ℃ of insulations 0.5 hour, be warmed up to 500～540 ℃ of insulations 1 hour at last;
Precursor transforms and shaping base pre-sintering process is: continue to be warming up to 900～1100 ℃ of insulations after 0.5 hour through the shaping base after the hot degreasing, be warming up to 1300～1500 ℃ and be incubated 1 hour then.
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| WO2018013991A3 (en) * | 2016-07-15 | 2018-02-22 | Oned Material Llc | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
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| CN104119094B (en) * | 2014-08-08 | 2016-03-02 | 苏州宏久航空防热材料科技有限公司 | Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof |
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Patent Citations (4)
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| US4801510A (en) * | 1987-09-02 | 1989-01-31 | Kennametal Inc. | Alumina coated silcon carbide whisker-alumina composition |
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| WO2018013991A3 (en) * | 2016-07-15 | 2018-02-22 | Oned Material Llc | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| US10862114B2 (en) | 2016-07-15 | 2020-12-08 | Oned Material Llc | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
| US11728477B2 (en) | 2016-07-15 | 2023-08-15 | Oned Material, Inc. | Manufacturing apparatus and method for making silicon nanowires on carbon based powders for use in batteries |
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