CN106957180B - Cf/C-SiC composite material and preparation method and application thereof - Google Patents

Cf/C-SiC composite material and preparation method and application thereof Download PDF

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CN106957180B
CN106957180B CN201710141633.8A CN201710141633A CN106957180B CN 106957180 B CN106957180 B CN 106957180B CN 201710141633 A CN201710141633 A CN 201710141633A CN 106957180 B CN106957180 B CN 106957180B
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CN106957180A (en
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孙少伟
欧阳晓平
齐福刚
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Xiangtan University
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Abstract

The composite material designed by the invention comprises a carbon fiber preform, matrix carbon, a filler and diamond-like carbon; the matrix carbon is uniformly attached to the carbon fiber of the prefabricated body to form the carbon fiber prefabricated body with the matrix carbon; the filler is filled in the carbon fiber prefabricated part with the matrix carbon and coated outside the carbon fiber prefabricated part with the matrix carbon to form a semi-finished product, and the diamond-like carbon is coated on the semi-finished product to form a diamond-like carbon layer; the filler contains Ti element, Si element, C element and Mo element. The invention adopts a method combining four processes of CVI + SI + RMI + PECVD to prepare a finished product with the advantages of high density, small thermal expansion coefficient, small friction coefficient, high self-lubricity, high thermal conductivity, oxidation resistance, thermal shock resistance, ablation resistance, wear resistance, high strength, high toughness and the like.

Description

Cf/C-SiC composite material and preparation method and application thereof
Technical Field
The invention belongs to the field of mechanical materials, and particularly relates to a Cfa/C-SiC composite material and a preparation method and application thereof.
Background
The piston is the 'heart' of an automobile engine, bears alternating mechanical load and thermal load, and is one of the most severe key parts in the engine under the worst working conditions. The piston functions to withstand the gas pressure and is transmitted by a piston pin to a connecting rod to drive the crankshaft in rotation, the piston crown also being part of the combustion chamber. With the rapid development of the automobile industry, the requirements of high-end sports cars such as faradi, lanbokini and the like on the heart are more and more strict. In order to prolong the service life of the piston and improve the safety of the piston in use, various profiled structures have to be designed and advanced coating treatment techniques have to be adopted. In fact, in practical application, the design of the special-shaped outer circle composite molded surface, the special-shaped pin hole and other structures often makes the structural design of the part complicated, increases the difficulty of processing, and increases the development and use cost. Even if various advanced coating treatment technologies are developed for the cast iron piston and the aluminum alloy piston which are used before, the working conditions of high rotating speed, high pressure and high thermal shock of the cast iron piston and the aluminum alloy piston can not be met obviously, and the cost for developing and producing the coating with long period and high cost is very much for manufacturers. Recently, related companies and enterprises have proposed a carbon fiber piston, namely a piston made of carbon fiber reinforced carbon-based composite material, which comprises a head part, a skirt part and a pin boss. However, at present, the piston is not put into production, and the marketization of the piston is not seen, mainly because a complete and specific carbon fiber piston production and preparation process route does not exist at present, and in addition, the pure carbon/carbon composite material has inherent defects of poor high-temperature mechanical property, poor heat conduction capability, easiness in soft deformation and the like, and the preparation period is long, so that the large-scale production is difficult, and high requirements are put forward on the modification preparation and process method of the carbon/carbon composite material.
Thus, a unique, low cost, short cycle C was soughtfThe preparation process of the/C-SiC composite material is characterized in that the pure carbon/carbon composite material is modified by doping the filler, so that the carbon fiber piston with excellent quality is prepared, and in addition, the coating which is practical, effective and low in cost is added, so that the scale production and the market expansion of the carbon fiber piston can be accelerated.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a Cfa/C-SiC composite material and a preparation method and application thereof.
The invention relates to afthe/C-SiC composite material comprises a carbon fiber preform, matrix carbon, a filler and diamond-like carbon; the matrix carbon is uniformly attached to the carbon fiber of the prefabricated body to form a carbon fiber prefabricated body with the matrix carbon; the filler is filled in the carbon fiber prefabricated part with the matrix carbon and coated outside the carbon fiber prefabricated part with the matrix carbon to form a semi-finished product, and the diamond-like carbon is coated on the semi-finished product to form a diamond-like carbon layer; the filler contains Ti element, Si element, C element and Mo element; ti element in the filler is selected from one or two of titanium carbide and silicon-carbon-titanium(ii) present; si element in the filler exists in at least one mode of SiC, simple substance Si, silicon carbon titanium and molybdenum silicide; c element in the filler exists in the form of at least one of SiC, silicon carbon titanium and silicon carbon titanium; the Mo element in the filler exists in the form of at least one of zero-valent molybdenum, molybdenum silicide and molybdenum carbide.
As a preferred embodiment, the invention relates to CfThe Si element in the filler exists in a mode of blending at least one of silicon, carbon, titanium and molybdenum silicide with SiC and simple substance Si.
The invention relates to afa/C-SiC composite material, said Cfthe/C-SiC composite material contains silicon carbon titanium (Ti)3SiC2) Phase, molybdenum silicide (MoSi)2) Phase, molybdenum carbide (Mo)2C) And (4) phase(s).
The invention relates to afSelecting a semi-finished product with the mass of B, measuring the sum of the masses of Ti element and Mo element in the semi-finished product, and defining the sum as A, wherein A/B is 0.04-0.08. Preferably, a/B is 0.04 to 0.075. Further preferably, a/B is 0.045 to 0.075.
The invention relates to afThe mass ratio of titanium to Mo of the/C-SiC composite material is 0.6-1.04: 1. Preferably 0.65-0.68: 1.
The invention relates to afThe density of the carbon fiber preform is 0.5-0.6g/cm3。
The invention relates to afThe density of a carbon fiber preform with matrix carbon is 1.3-1.4 g/cm3。
The invention relates to afThe density of a semi-finished product of the/C-SiC composite material is 1.8-1.9 g/cm3。
The invention relates to afa/C-SiC composite material, said CfThe density of the/C-SiC composite material is 1.82-1.92 g/cm3. In the present invention, said CfThe density of the/C-SiC composite material is greater than that of the semi-finished product.
The invention relates to afThe preparation method of the/C-SiC composite material comprises the following steps:
step one
Weaving carbon fibers into a prefabricated body, and then carrying out chemical vapor infiltration deposition on matrix carbon; the obtained density is 1.3-1.4 g/cm3The carbon fiber preform with matrix carbon of (a); the density of the prefabricated body is 0.5-0.6g/cm3；
Step two
Dipping the carbon fiber preform with the matrix carbon obtained in the step one in dipping liquid containing Ti and Mo to obtain a preform containing Ti and Mo;
step three
Placing the prefabricated body containing Ti and Mo obtained in the step two on Si powder or embedding the prefabricated body in the Si powder, and carrying out siliconizing treatment at the temperature of 1500-; the obtained density is 1.8-1.9 g/cm3The semi-finished product of (2);
step four
Coating a diamond-like carbon layer on the surface of the semi-finished product obtained in the step three; and obtaining a finished product.
The invention relates to afIn the first step, the carbon fiber is mesophase pitch-based carbon fiber. Compared with polyacrylonitrile-based carbon fibers, the mesophase pitch-based carbon fibers are cheap and easy to obtain; compared with viscose-based carbon fiber, the mechanical property is excellent, and the weaving is easy; more importantly, the heat conductivity of the mesophase pitch-based carbon fiber is better than that of polyacrylonitrile-based carbon fiber and viscose-based carbon fiber.
The invention relates to afIn the first step, the preform is a three-dimensional four-way or three-dimensional five-way needling carbon felt porous preform. Compared with one-dimensional, two-dimensional and 2.5-dimensional knitting processes, the three-dimensional four-way or three-dimensional five-way needle-punched knitted fabric has the advantages that the integrity of the knitted fabric is obviously improved, the volume fraction of fibers in the thickness direction of the material is obviously improved, and the interlaminar shear strength and the rigidity in the thickness direction of the material can be effectively improved. And no layering occurs from weaving and compounding to a finished product, no mechanical processing is performed or only a small amount of processing which does not damage the porous preform of the carbon fiber piston is performed, and the integrity of the material is maintained.
The invention relates to afThe preparation method of the/C-SiC composite material comprises the step one, when matrix carbon is deposited by chemical vapor infiltrationThe carbon source gas is at least one of propane, ethylene and acetylene. Propane is preferred. The method has the advantages of easy acquisition of materials, mature process, convenient operation and lower preparation cost, can prepare the carbon matrix with excellent high-temperature mechanical property, and ensures that the infiltrated carbon matrix is compact and uniform and has few cracks.
The invention relates to afIn the first step, when matrix carbon is deposited by chemical vapor infiltration, the used diluent gas is at least one of argon and nitrogen. Argon is preferred.
The invention relates to afIn the first step, when matrix carbon is subjected to chemical vapor infiltration deposition, the gas inlet speed of a carbon source gas is 0.5-0.9L/min, preferably 0.7L/min; the inlet velocity of the diluent gas is 2.5-3.3L/min, preferably 3L/min.
The invention relates to afThe preparation method of the/C-SiC composite material comprises the following steps that in the first step, when matrix carbon is subjected to chemical vapor infiltration deposition, the heating rate is controlled to be 5-6 ℃/min; the deposition temperature is controlled to be 1000-1100 ℃, and the preferred temperature is 1000 ℃; and controlling the heat preservation time to be 450-600 h at the deposition temperature.
The method only needs about 500 hours, and deposits a part of compact and uniform carbon matrix to ensure that the density of the carbon matrix is 1.3-1.4 g/cm3In between, appropriate voids remain in the carbon/carbon preform. The process method can shorten the preparation period, save the cost and is also beneficial to the impregnation of the slurry later. When the carbon matrix content is too high, the dispersion is uneven, the performance is reduced, gaps are filled, the slurry is difficult to soak, and the purpose of modifying the doped filler is difficult to realize; when the content is too low, the effect of the carbon fiber cannot be fully exerted, and the performance of the material cannot be obviously improved. Therefore, a large number of tests prove that the carburizing time of the porous preform of the carbon fiber piston is preferably 500-600 h, so that the density of the carbon/carbon preform is 1.3-1.4 g/cm3In the meantime.
The invention relates to afThe preparation method of the/C-SiC composite material comprises the second step,
putting the carbon fiber preform with the matrix carbon obtained in the step one into dipping liquid containing Ti and Mo for vacuum dipping, and drying after vacuum dipping to obtain a preform containing Ti and Mo; the Ti and Mo-containing immersion liquid is prepared from water, micron titanium carbide (TiC), micron molybdenum (Mo) and CMC (sodium carboxymethylcellulose) in a mass ratio of water: micron titanium carbide (TiC): micron molybdenum (Mo): CMC (sodium carboxymethylcellulose) ═ 100-90:50-55:60-65:0.5-0.8, preferably 100: 50: 60: 0.8; and during vacuum impregnation, the air pressure in the equipment is less than or equal to 13.33 Pa.
In the industrial application, the materials are fully ground for 25 to 30 hours by an electronic pulp machine after being mixed, so that the materials are fully and uniformly dispersed. Then the obtained product is sent into a vacuum impregnation tank, and the vacuum impregnation tank is vacuumized to be less than the limit residual pressure of 13.33 Pa. During vacuum impregnation, most of the water is removed. The moisture plays a role in transportation in the dipping process, and after the moisture transports the micron titanium carbide (TiC) and the micron molybdenum (Mo) into the prefabricated body, the moisture can be quickly separated from the prefabricated body. Therefore, after the carbon/carbon composite material is impregnated, the carbon/carbon composite material can be dried in the shade or baked at low temperature to obtain the impregnated carbon/carbon preform.
The granularity of the micron titanium carbide is 20-50 microns; the particle size of the micron molybdenum is 20-50 microns.
In order to ensure that the micron titanium carbide (TiC) and the micron molybdenum (Mo) can be fully impregnated into the carbon/carbon porous preform, the vacuum impregnation time is preferably 25-32h, and if the vacuum impregnation time is too long, the preparation efficiency is influenced, the energy is wasted, and the improvement of the material performance is not greatly influenced. A large number of tests prove that the introduced micron titanium carbide and micron molybdenum account for 6 to 9 percent of the mass of the carbon/carbon preform after the whole infiltration.
Preferably, the impregnation process is vacuum impregnation. The impregnation slurry prepared by the mixture of distilled water, micron titanium carbide (TiC), micron molybdenum (Mo) and CMC (sodium carboxymethylcellulose) has good wettability with a carbon matrix, a small contact angle and large impregnation pressure, can be impregnated under normal pressure, obviously, the impregnation rate can be accelerated by adopting vacuum impregnation, and the preparation period can be shortened. And vacuum pressure infiltration is not adopted, because the carbon/carbon prefabricated part which is not completely formed can be damaged during pressure, so that the carbon/carbon prefabricated part is slightly deformed.
The invention relates to afThe preparation method of the/C-SiC composite material comprises the third step,
placing the prefabricated body containing Ti and Mo obtained in the step two on Si powder or embedding the prefabricated body in the Si powder, and carrying out siliconizing treatment at the temperature of 1500-; the obtained density is 1.8-1.9 g/cm3And (4) semi-finished products of the product.
Preferably, the pressure in the furnace is 3 to 6Pa in a vacuum atmosphere.
As a preferred scheme, in the third step, the vacuum reaction furnace is vacuumized, and the furnace pressure is still less than 3-6 Pa; then, the furnace temperature is increased to 1500 ℃ within 7-8 h, and the temperature is kept for 5 h; then the furnace temperature is increased to 1750 ℃ by 1h, and the temperature is kept for 0.5 h; finally, argon is used as protective gas, the pressure of the argon is controlled to be 2.5KPa, and the furnace is cooled.
According to the invention, during siliconizing treatment in the third step, good wettability and small contact angle are formed between the molten silicon and the carbon, the titanium carbide and the molybdenum, and the high vacuum process is favorable for increasing the infiltration speed of the molten silicon, accelerating the reaction rate with the carbon matrix and the filler, and is favorable for the generation of silicon carbide ceramics, silicon carbon titanium and molybdenum silicide and the like. The elimination of pressure siliconizing also takes into account that the initial stage of siliconizing may cause damage to the carbon/carbon piston preform, resulting in stress strain. And a precursor impregnation cracking method is not adopted for preparing the silicon carbide substrate, so that the preparation period is obviously shortened, and the cost is saved. Meanwhile, by adopting the vacuum reaction melting siliconizing process designed by the invention, the prepared silicon carbide ceramic matrix completely meets the application of products in special fields (such as high pressure resistance, high temperature resistance and thermal shock resistance required by pistons).
The invention relates to afThe preparation method of the/C-SiC composite material comprises the fourth step,
placing the semi-finished product obtained in the step three in a deposition furnace, and depositing and coating the diamond-like carbon layer by adopting a plasma deposition technology; when the plasma deposition technology is used for depositing the diamond-like carbon layer, the pressure in the furnace is controlled to be 3-13.33Pa, preferably 5Pa, the deposition temperature is controlled to be 60-80 ℃, the deposition power is controlled to be 600-620W, and the gas used for deposition is CH4And H2The flow rates are 2, respectively.1-2.4mL/min and 6.4-6.9mL/min, and the deposition time is 15-16 h.
Preferably, the thickness of the diamond-like coating is 8-10 μm. The deposition time is too long, so that the thickness of the coating is too large, the heat conduction is not facilitated, and when the coating is used as a piston, the throat of the piston is easy to ablate, so that the coating is greatly peeled off. Too short a deposition time and too thin a coating layer will not have the effect of thermal ablation resistance.
In application, the A/B value of the obtained material is controlled by controlling the density of the carbon fiber preform with matrix carbon obtained in the step one, controlling the dosage of micron titanium carbide (TiC) and micron molybdenum (Mo) in the slurry in the step two, and matching the dipping condition with the temperature, time and other conditions of melt Si dipping in the step three.
According to the invention, because the surface of the prepared carbon fiber piston is always provided with Si residues, the Si can inhibit the graphitization of the DLC coating, the thin silicon oxide layer on the surface of the coating plays a role in inhibiting oxidation or rapid heat conduction, the thermal stability and the wear resistance of the DLC coating are greatly improved, and the DLC coating has a unique function of friction reduction and wear resistance and is very in line with the working condition requirements of the piston. In addition, the methane is used as a precursor of the DLC coating, the material is easy to obtain, the operation is convenient, the preparation cost is low, the DLC coating with excellent high-temperature mechanical property can be prepared, and the prepared coating has strong binding force with the prepared inner surface, is uniform and compact, is not easy to fall off, and has excellent effect.
The invention relates to afThe application of the/C-SiC composite material comprises the application of the/C-SiC composite material as a piston. When the carbon fiber is used as a piston, only carbon fiber is woven into a piston-shaped prefabricated body; other operations were performed according to the protocol described in the present invention.
The invention relates to afThe application of the/C-SiC composite material also comprises the application in the fields of spaceflight, military industry, civil use and the like.
Principles and advantages
The invention adopts a method combining four processes of Chemical Vapor Infiltration (CVI), Slurry Infiltration (SI), vacuum Reaction Melt Infiltration (RMI) and Plasma Enhanced Chemical Vapor Deposition (PECVD), and two fillers of micron titanium carbide (TiC) and micron molybdenum (Mo) are doped in the slurry,and preparing a finished product. The method comprises the steps of weaving a three-dimensional four-way or three-dimensional five-way needled carbon felt porous preform by using mesophase pitch-based carbon fibers, depositing carbon by adopting a CVI (chemical vapor infiltration) method, and filling small pores in a fiber bundle of the porous preform to form the carbon/carbon preform. The mixture of water, micron titanium carbide (TiC), micron molybdenum (Mo) and CMC (sodium carboxymethyl cellulose) is used as dipping slurry, and the carbon/carbon piston preform is vacuum dipped by the SI method, so that two fillers of micron titanium carbide (TiC) and micron molybdenum (Mo) are introduced into the carbon/carbon preform. And then melting and siliconizing the carbon/carbon piston preform by an RMI method, thereby preparing the carbon fiber piston containing the carbon-silicon carbide double matrix. And finally, depositing a DLC coating on the surface of the carbon fiber piston by adopting a PECVD method. The mesophase pitch-based carbon fiber is selected as the raw material of the woven preform, and the mesophase pitch-based carbon fiber has the advantages of high heat conductivity, high modulus, easy graphitization and more important low cost. The reason why the needled carbon felt preform which is knitted into the three-dimensional four-direction or three-dimensional five-direction is that the excellent mechanical properties of the carbon fibers in all directions can be easily exerted by the knitted structure. The two points already lay a firm foundation for high heat conduction and high strength after molding. And then when the carbon matrix is deposited by adopting a CVI method, the carbon fiber is not easy to be damaged, and the later perfect performance of the composite material is ensured. Titanium carbide (TiC) and micron molybdenum (Mo) are added into the dipping slurry of the slurry infiltration method as fillers, and because the volume and the mass of the fillers are not changed, the shrinkage of a carbon matrix can be inhibited to a certain degree, so that the material is rapidly densified, and the preparation period is shortened. And then siliconizing the carbon/carbon piston preform doped with micron TiC and micron Mo by adopting an RMI method to generate a large amount of silicon carbide ceramic hard matrixes, wherein the piston prepared from the carbon fiber reinforced carbon and silicon carbide double-matrix composite material has the advantages of low density, good oxidation resistance, corrosion resistance, wear resistance, excellent mechanical property, excellent thermophysical property and the like. At the same time, when a small amount of silicon carbon titanium (Ti) is generated3SiC2) Molybdenum silicide (MoSi)2) Molybdenum carbide (Mo)2C) When in the same phase, these phases formed can be strengthened by particle dispersion in the matrix and synergistically enhance the flexural strength and fracture resistance of the overall composite material preparation with the matrixThe toughness and the generated phase also have the good characteristics of self-healing damage mechanism, self-lubrication, low friction coefficient and the like, and are very suitable for the working condition of the piston. Meanwhile, the developed material has better plasticity, which is beneficial to the processing and forming of the piston. Finally, the piston is plated with the DLC coating by adopting a PECVD method. The DLC is plated, because the surface of the prepared carbon fiber piston is bound to have Si residues, the Si can inhibit the graphitization of the DLC coating, the thin-layer silicon oxide on the surface of the coating plays a role in inhibiting oxidation or rapid heat conduction, the thermal stability and the wear resistance of the DLC coating are greatly improved, and the DLC coating has the unique functions of friction reduction and wear resistance and is very in line with the working condition requirements of the piston.
In a word, the invention designs a material with excellent performance and explores a complete process route for preparing the carbon fiber by modifying the doping filler. Especially, the whole process for preparing the piston is simple, the period is short, the equipment requirement is simple, the cost is low, the net forming of the piston can be realized, the prepared piston can meet the harsh working conditions of high pressure, high rotating speed and high thermal shock, and the service life of the piston is much longer than that of a common piston under continuous cycle work.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the technical solution of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below.
Fig. 1 is a flow chart of a manufacturing process method according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby. It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Example 1
As shown in fig. 1, a method for preparing a silicon carbide fiber reinforced silicon carbide ceramic matrix composite according to an embodiment of the present invention includes the following steps:
step 1, preparing a carbon fiber piston porous preform:
weaving carbon fibers into a piston-shaped prefabricated body by adopting a knitting process; the carbon fiber in the porous preform of the carbon fiber piston is mesophase pitch-based carbon fiber. The density of the piston-shaped preform is 0.58g/cm3(ii) a The prefabricated body is a three-dimensional five-direction needling carbon felt porous prefabricated body;
step 2, preparing a carbon/carbon piston preform:
and placing the carbon fiber piston porous preform in a tool mold by adopting a chemical vapor infiltration method, and then placing the carbon fiber piston porous preform and the tool mold into a chemical vapor deposition furnace together. Carbon is infiltrated on the carbon fiber piston preform obtained in the step 1 through a carbon organic matter precursor, and the prepared carbon fiber piston preform with the density of 1.34g/cm3The carbon/carbon piston preform of (1); when the chemical vapor infiltration deposition matrix carbon is adopted, the used carbon source gas is propane, the used diluent gas is argon, and when the chemical vapor infiltration deposition matrix carbon is adopted, the gas inlet speed of the carbon source gas is 0.7L/min; the inlet velocity of the diluent gas was 0.18Nm3H (i.e., 3L/min). Controlling the heating rate to be 5.6 ℃/min when the chemical vapor infiltration deposits the matrix carbon; controlling the deposition temperature to be 1000 ℃; and controlling the heat preservation time to be 560h at the deposition temperature.
Step 3, preparing a slurry carburized/carbon piston preform:
putting the carbon/carbon piston preform obtained in the step 2 into dipping liquid containing Ti and Mo for vacuum dipping to obtain a preform containing Ti and Mo; the impregnation liquid containing Ti and Mo is prepared from water, micron titanium carbide (TiC), micron molybdenum (Mo) and CMC (sodium carboxymethylcellulose) in a mass ratio of water: micron titanium carbide (TiC): micron molybdenum (Mo): CMC (sodium carboxymethylcellulose) ═ 100: 50: 60: 0.8; and during vacuum impregnation, the air pressure in the equipment is less than or equal to 13.33 Pa. The granularity of the micron titanium carbide is 30 microns; the particle size of the micron molybdenum is 30 microns. The vacuum impregnation time was 27 h. Drying after vacuum impregnation is finished; obtaining a prefabricated body containing Ti and Mo; the micron titanium carbide and the micron molybdenum which are introduced after the vacuum impregnation are 7 percent of the dry weight of the whole preform containing Ti and Mo.
The preparation method of the impregnation liquid comprises the following steps:
after the materials are mixed, the materials are fully ground for 25 to 30 hours by an electronic pulp machine, so that the materials are fully and uniformly dispersed. Then the mixture is sent into a vacuum impregnation tank, and the vacuum impregnation tank is vacuumized to be less than the limit residual pressure of 13.33 Pa.
Step 4, preparing the carbon fiber piston containing the carbon-silicon carbide matrix:
placing the prefabricated body containing Ti and Mo obtained in the step 3 on Si powder or embedding the prefabricated body in the Si powder, and carrying out siliconizing treatment at 1500 ℃ in a vacuum atmosphere; the density obtained was 1.89g/cm3And (4) semi-finished products of the product.
Before siliconizing, vacuumizing a vacuum reaction furnace, and still keeping the furnace pressure less than 3-6 Pa; then, the furnace temperature is increased to 1500 ℃ within 7h, and the temperature is kept for 5 h; then the furnace temperature is increased to 1750 ℃ by 1h, and the temperature is kept for 0.5 h; finally, argon is used as protective gas, the pressure of the argon is controlled to be 2.5KPa, and the furnace is cooled.
Step 5, preparing a carbon fiber piston surface coating:
and (3) putting the semi-finished product obtained in the step (4) into plasma chemical vapor deposition equipment by adopting a plasma enhanced chemical vapor deposition method, and depositing the ionized carbon organic matter precursor on the surface of the semi-finished product to obtain the DLC (diamond-like carbon) coating. When the plasma deposition technology is used for depositing the diamond-like carbon layer, the pressure in the furnace is controlled to be 5Pa, the deposition temperature is controlled to be 60-80 ℃, the deposition power is 600W, and the gas used for deposition is CH4And H2The flow rates of the two are respectively 2.1mL/min and 6.4mL/min, and the deposition time is 15-16 h; the finished product with the diamond-like coating thickness of 9 μm is obtained. The properties of the finished product are shown in Table 1
TABLE 1 Performance parameters of carbon fiber pistons prepared by the present invention
Figure BDA0001242987450000121
Example 2
Step 1, preparing a carbon fiber piston porous preform:
weaving carbon fibers into a piston-shaped prefabricated body by adopting a knitting process; the carbon fiber in the porous preform of the carbon fiber piston is mesophase pitch-based carbon fiber. The density of the piston-shaped preform is 0.6g/cm3(ii) a The prefabricated body is a three-dimensional five-direction needling carbon felt porous prefabricated body;
step 2, preparing a carbon/carbon piston preform:
and placing the carbon fiber piston porous preform in a tool mold by adopting a chemical vapor infiltration method, and then placing the carbon fiber piston porous preform and the tool mold into a chemical vapor deposition furnace together. Carbon is infiltrated on the carbon fiber piston preform obtained in the step 1 through a carbon organic matter precursor, and the prepared carbon fiber piston preform with the density of 1.38g/cm3The carbon/carbon piston preform of (1); when the chemical vapor infiltration deposition matrix carbon is adopted, the used carbon source gas is propane, the used diluent gas is argon, and when the chemical vapor infiltration deposition matrix carbon is adopted, the gas inlet speed of the carbon source gas is 0.8L/min; the inlet velocity of the diluent gas was 3.3L/min. Controlling the heating rate to be 5.5 ℃/min when the chemical vapor infiltration deposits the matrix carbon; controlling the deposition temperature to be 1000 ℃; the incubation time was controlled at the deposition temperature for 550 h.
Step 3, preparing a slurry carburized/carbon piston preform:
putting the carbon/carbon piston preform obtained in the step 2 into dipping liquid containing Ti and Mo for vacuum dipping to obtain a preform containing Ti and Mo; the impregnation liquid containing Ti and Mo is prepared from water, micron titanium carbide (TiC), micron molybdenum (Mo) and CMC (sodium carboxymethylcellulose) in a mass ratio of water: micron titanium carbide (TiC): micron molybdenum (Mo): CMC (sodium carboxymethylcellulose) ═ 100: 50: 60: 0.8; and during vacuum impregnation, the air pressure in the equipment is less than or equal to 13.33 Pa. The granularity of the micron titanium carbide is 50 microns; the micron molybdenum has a particle size of 50 microns. The vacuum impregnation time is 24h, 25h, 27h, 29h, 32h and 36 h. After vacuum impregnation is finished, obtaining a prefabricated body containing Ti and Mo; the micron titanium carbide and the micron molybdenum introduced after the vacuum impregnation are 5%, 6%, 7%, 8%, 9%, 10% and the like of the whole preform mass containing Ti and Mo.
The preparation method of the impregnation liquid comprises the following steps:
after the materials are mixed, the materials are fully ground for 25 to 30 hours by an electronic pulp machine, so that the materials are fully and uniformly dispersed. Then the mixture is sent into a vacuum impregnation tank, and the vacuum impregnation tank is vacuumized to be less than the limit residual pressure of 13.33 Pa.
Step 4, preparing the carbon fiber piston containing the carbon-silicon carbide matrix:
placing the prefabricated body containing Ti and Mo obtained in the step 3 on Si powder or embedding the prefabricated body in the Si powder, and carrying out siliconizing treatment at 1750 ℃ in a vacuum atmosphere; the density obtained was 1.88g/cm3And (4) semi-finished products of the product.
Before siliconizing, vacuumizing a vacuum reaction furnace, and still keeping the furnace pressure less than 3-6 Pa; then, the furnace temperature is increased to 1500 ℃ within 7h, and the temperature is kept for 5 h; then the furnace temperature is increased to 1750 ℃ by 1h, and the temperature is kept for 0.5 h; finally, argon is used as protective gas, the pressure of the argon is controlled to be 2.5KPa, and the furnace is cooled.
Step 5, preparing a carbon fiber piston surface coating:
and (3) putting the semi-finished product obtained in the step (4) into plasma chemical vapor deposition equipment by adopting a plasma enhanced chemical vapor deposition method, and depositing the ionized carbon organic matter precursor on the surface of the semi-finished product to obtain the DLC (diamond-like carbon) coating. When the plasma deposition technology is used for depositing the diamond-like carbon layer, the pressure in the furnace is controlled to be 5Pa, the deposition temperature is controlled to be 60-80 ℃, the deposition power is 600W, and the gas used for deposition is CH4And H2The flow rates of the two are respectively 2.1mL/min and 6.4mL/min, and the deposition time is 15-16 h; the finished product with the thickness of the diamond-like coating of 10 mu m is obtained. The properties of the finished product are shown in Table 2
Through a large number of tests, four performance parameters which are most critical to the influence of the mass fraction of the doped filler on the performance of the piston are obtained, as shown in table 2:
TABLE 2 Effect of the mass fraction of doped Filler on piston Performance parameters
Figure BDA0001242987450000141
Example 3
Step 1, preparing a carbon fiber piston porous preform:
weaving carbon fibers into a piston-shaped prefabricated body by adopting a knitting process; the carbon fiber in the porous preform of the carbon fiber piston is mesophase pitch-based carbon fiber. The density of the piston-shaped preform is 0.58g/cm3(ii) a The prefabricated body is a three-dimensional five-direction needling carbon felt porous prefabricated body;
step 2, preparing a carbon/carbon piston preform:
and placing the carbon fiber piston porous preform in a tool mold by adopting a chemical vapor infiltration method, and then placing the carbon fiber piston porous preform and the tool mold into a chemical vapor deposition furnace together. Carbon is infiltrated on the carbon fiber piston prefabricated body obtained in the step 1 through a carbon organic matter precursor, and a carbon/carbon piston prefabricated body is prepared; when the matrix carbon is subjected to chemical vapor infiltration deposition, the used carbon source gas is propane, the used diluent gas is argon, and when the matrix carbon is subjected to chemical vapor infiltration deposition, the gas inlet speed of the carbon source gas is 0.8L/min; the inlet velocity of the diluent gas was 3L/min. Controlling the heating rate to be 5.6 ℃/min when the chemical vapor infiltration deposits the matrix carbon; controlling the deposition temperature to be 1100 ℃; the temperature holding time is controlled to be 550h at the deposition temperature.
Step 3, preparing a slurry carburized/carbon piston preform:
putting the carbon/carbon piston preform obtained in the step 2 into dipping liquid containing Ti and Mo for vacuum dipping to obtain a preform containing Ti and Mo; the impregnation liquid containing Ti and Mo is prepared from water, micron titanium carbide (TiC), micron molybdenum (Mo) and CMC (sodium carboxymethylcellulose) in a mass ratio of water: micron titanium carbide (TiC): micron molybdenum (Mo): CMC (sodium carboxymethylcellulose) ═ 100: 50: 60: 0.8; and during vacuum impregnation, the air pressure in the equipment is less than or equal to 13.33 Pa. The granularity of the micron titanium carbide is 20 microns; the particle size of the micron molybdenum is 20 microns. The vacuum impregnation time was 27 h. After vacuum impregnation is finished, obtaining a prefabricated body containing Ti and Mo; the micron titanium carbide and the micron molybdenum introduced after the vacuum impregnation are 5%, 6%, 7%, 8%, 9%, 10% and the like of the whole preform mass containing Ti and Mo.
The preparation method of the impregnation liquid comprises the following steps:
after the materials are mixed, the materials are fully ground for 30 hours by an electronic pulp machine, so that the materials are fully dispersed and uniform. Then the mixture is sent into a vacuum impregnation tank, and the vacuum impregnation tank is vacuumized to be less than the limit residual pressure of 13.33 Pa.
Step 4, preparing the carbon fiber piston containing the carbon-silicon carbide matrix:
placing the prefabricated body containing Ti and Mo obtained in the step 3 on Si powder or embedding the prefabricated body in the Si powder, and carrying out siliconizing treatment at 1500 ℃ in a vacuum atmosphere; the density obtained was 1.89g/cm3And (4) semi-finished products of the product.
Preferably, the pressure in the furnace is 3 to 6Pa in a vacuum atmosphere.
Siliconizing money, namely vacuumizing a vacuum reaction furnace at first, and still keeping the furnace pressure less than 3-6 Pa; then, the furnace temperature is increased to 1500 ℃ within 7h, and the temperature is kept for 5 h; then the furnace temperature is increased to 1750 ℃ by 1h, and the temperature is kept for 0.5 h; finally, argon is used as protective gas, the pressure of the argon is controlled to be 2.5KPa, and the furnace is cooled.
Step 5, preparing a carbon fiber piston surface coating:
and (3) putting the semi-finished product obtained in the step (4) into plasma chemical vapor deposition equipment by adopting a plasma enhanced chemical vapor deposition method, and depositing the ionized carbon organic matter precursor on the surface of the semi-finished product to obtain the DLC (diamond-like carbon) coating. When the plasma deposition technology is used for depositing the diamond-like carbon layer, the pressure in the furnace is controlled to be 10Pa, the deposition temperature is controlled to be 60-80 ℃, the deposition power is 600W, and the gas used for deposition is CH4And H2The flow rate of the second solution is 2.1mL/min and 6.4mL/min respectively, and the deposition time is 15-16 h; the finished product with the thickness of the diamond-like coating of 10 mu m is obtained.
The piston (finished products obtained in examples 1-3) prepared by the preparation method explored by the invention from the material selection, weaving, carbon deposition, filler impregnation and siliconizing to the coating of the piston passes through the mechanical fatigue test of the piston, and the pin hole runs for 10 times under the cycle pressure of 30MPa7The cycle of (2) is crack-free. Through a piston fatigue test, the top of the piston has no crack after 3000 times of cyclic thermal shock tests. The durability test of the engine in 1100 hours under the conditions of 4300rpm of the rotation speed of the engine and 30MPa of detonation pressure is met. The piston has self-lubricating and high-temperature self-healing damage mechanisms, completely meets the severe working condition of the piston, and has service life which can be improved by more than one time compared with a cast iron piston and an aluminum alloy piston.
In the description of the present invention, numerous specific details are set forth. It is understood, however, that embodiments of the invention may be practiced without these specific details. In some instances, well-known methods, structures and techniques have not been shown in detail in order not to obscure an understanding of this description.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications and the substitutions do not cause the essence of the corresponding technical solutions to depart from the scope of the technical solutions of the embodiments of the present invention, and the corresponding technical solutions are all covered in the claims and the specification of the present invention.

Claims (6)

1. CfThe preparation method of the/C-SiC composite material is characterized by comprising the following steps: said C isfthe/C-SiC composite material comprises a carbon fiber preform, matrix carbon, a filler and diamond-like carbon; the matrix carbon is uniformly attached to the carbon fiber of the prefabricated body to form the carbon fiber prefabricated body with the matrix carbon; the filler is filled in the carbon fiber prefabricated part with the matrix carbon and coated outside the carbon fiber prefabricated part with the matrix carbon to form a semi-finished product, and the diamond-like carbon is coated on the semi-finished product to form a diamond-like carbon layer; the filler contains Ti element, Si element, C element and Mo element; the Ti element in the filler exists in any one or two modes of titanium carbide and silicon carbon titanium; the Si element in the filler is SiC, simple substance Si, silicon carbon titanium and molybdenum silicideAt least one means exists; c element in the filler exists in the form of at least one of SiC and silicon carbon titanium; the Mo element in the filler exists in the form of at least one of zero-valent molybdenum, molybdenum silicide and molybdenum carbide;
said C isfthe/C-SiC composite material is prepared by the following steps:
step one
Weaving carbon fibers into a prefabricated body, and then carrying out chemical vapor infiltration deposition on matrix carbon; the obtained density is 1.3-1.4 g/cm3The carbon fiber preform with matrix carbon of (a); the density of the prefabricated body woven by the carbon fibers is 0.5-0.6g/cm3；
Step two
Putting the carbon fiber preform with the matrix carbon obtained in the step one into dipping liquid containing Ti and Mo for vacuum dipping; the impregnation liquid containing Ti and Mo is prepared from water, micron titanium carbide, micron molybdenum and CMC in a mass ratio of water: micron titanium carbide: micron molybdenum: CMC =100-90:50-55:60-65: 0.5-0.8; during vacuum impregnation, the air pressure in the equipment is less than or equal to 13.33 Pa; the vacuum impregnation time is 25-32 h; the granularity of the micron titanium carbide is 20-50 microns; the granularity of the micron molybdenum is 20-50 microns; after vacuum impregnation is finished, drying to obtain a prefabricated body containing Ti and Mo; the introduced micron titanium carbide and micron molybdenum account for 6-9% of the mass of the whole infiltrated carbon/carbon preform;
step three
Placing the prefabricated body containing Ti and Mo obtained in the step two on Si powder or embedding the prefabricated body in the Si powder, and carrying out siliconizing treatment at the temperature of 1500-; the obtained density is 1.8-1.9 g/cm3The semi-finished product of (2);
step four
Placing the semi-finished product obtained in the step three in a deposition furnace, and depositing and coating the diamond-like carbon layer by adopting a plasma deposition technology; when the plasma deposition technology is used for depositing the diamond-like carbon layer, the pressure in the furnace is controlled to be 3-13.33Pa, the deposition temperature is controlled to be 60-80 ℃, the deposition power is controlled to be 600-620W, and the gas used for deposition is CH4And H2The flow rates of the two are respectively 2.1-2.4mL/min and 6.4-6.9mL/min, and the deposition time is 15-16 h; the thickness of the diamond-like coating is 8-10 mu m.
2. A compound C according to claim 1fThe preparation method of the/C-SiC composite material is characterized by comprising the following steps: said C isfthe/C-SiC composite material contains a silicon carbon titanium phase, a molybdenum silicide phase and a molybdenum carbide phase.
3. A compound C according to claim 1fThe preparation method of the/C-SiC composite material is characterized by comprising the following steps: selecting a semi-finished product with the mass of B, measuring the sum of the masses of Ti element and Mo element in the semi-finished product, and defining the sum as A, wherein A/B = 0.04-0.08.
4. A compound C according to claim 1fThe preparation method of the/C-SiC composite material is characterized by comprising the following steps: said C isfThe density of the/C-SiC composite material is 1.82-1.92 g/cm3。
5. A compound C according to claim 1fThe preparation method of the/C-SiC composite material is characterized by comprising the following steps:
in the first step, the carbon fiber is mesophase pitch-based carbon fiber;
in the first step, the prefabricated body woven by the carbon fibers is a three-dimensional four-way or three-dimensional five-way needling carbon felt porous prefabricated body;
in the first step, when matrix carbon is subjected to chemical vapor infiltration deposition, a carbon source gas is selected from at least one of propane and ethylene acetylene;
in the first step, when the matrix carbon is subjected to chemical vapor infiltration deposition, the used diluent gas is selected from at least one of argon and nitrogen;
in the first step, when the matrix carbon is subjected to chemical vapor infiltration deposition, the gas inlet speed of the carbon source gas is 0.5-0.9L/min; the gas inlet speed of the diluent gas is 2.5-3.3L/min;
in the first step, when the carbon of the matrix is subjected to chemical vapor infiltration deposition, the heating rate is controlled to be 5-6 ℃/min; the deposition temperature is controlled to be 1000-1100 ℃; and controlling the heat preservation time to be 450-600 hours at the deposition temperature.
6. A compound C according to claim 1fThe preparation method of the/C-SiC composite material is characterized by comprising the following steps: in the third step, the vacuum reaction furnace is vacuumized to ensure that the furnace pressure is 3-6 Pa; then, the furnace temperature is increased to 1500 ℃ within 7-8 h, and the temperature is kept for 5 h; then the furnace temperature is increased to 1750 ℃ by 1h, and the temperature is kept for 0.5 h; finally, argon is used as protective gas, the pressure of the argon is controlled to be 2.5KPa, and the furnace is cooled.
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