CN109650903A - A kind of carbon solid solution nitriding silicon materials and preparation method thereof - Google Patents
A kind of carbon solid solution nitriding silicon materials and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to material science and technology fields, and in particular to a kind of carbon solid solution nitriding silicon materials and preparation method thereof.The present invention is dissolved carbon in silicon nitride with mechanical alloying and self-propagating reaction method to regulate and control the chemical bond in silicon nitride, the carbon solid solution nitriding silicon materials of preparation are covalent bond and metallic bond mixed type, the performance degradation caused by the silicon nitride/silicon carbide fiber interface in traditional material microstructure is avoided, achievees the purpose that the mechanical performance and wear-resisting property of strengthening silicon nitride ceramic material.Carbon solid solution nitriding silicon materials of the present invention have many advantages, such as crystallinity height, high tenacity, resist wear-resisting, lightweight；In high speed ceramic bearing, the fields such as anticorrosive ceramic coating have a wide range of applications.
Description
Technical field
The invention belongs to material science and technology fields, and in particular to a kind of carbon solid solution nitriding silicon materials and preparation method thereof.
Background technique
Silicon nitride ceramic material has a wide range of applications as important structural material and functional material.But due to its material
The hardness of material is low, generally requires the mechanical performance that silicon nitride is improved by addition hard phase material.Currently, carbonization is widely used
Silica fibre adds to enhance the deficiency of silicon nitride ceramic material.Silicon carbide fibre depends on to enhance the performance of silicon nitride ceramics
The size of interface property and silicon carbide fibre between silicon carbide fibre and silicon nitride matrix, shape and in silicon nitride matrix
Distribution, this make by existing method obtain flexible silicon nitride it is very sensitive to preparation process, the stability kimonos of performance
The reliability of labour is all very poor.
Summary of the invention
In view of this, solving current silicon nitride it is an object of the invention to overcome technological deficiency existing in the prior art
The problem of Strengthening and Toughening deficiency provides a kind of carbon solid solution nitriding silicon materials and preparation method thereof, the carbon prepared using the method for the present invention
Solid solution nitriding silicon ceramic material has good fracture toughness and wear-resisting property.
Above-mentioned purpose that the invention is realized by the following technical scheme, the present invention provides a kind of carbon solid solution nitriding silicon materials
Preparation method, comprising the following steps:
(1) silicon powder, beta-silicon nitride powder, carbon black and ammonium chloride are uniformly mixed and are placed in ball grinder, it is close after addition dehydrated alcohol
Blocking grinding jar extracts after the air in tank is filled with high-purity inert nitrogen and carries out ball milling；
(2) dry in infrared drying oven after ball milling, Al is added in the powder after drying2O3And Y2O3Compressing tablet process after mixing；
(3) be placed in self-propagating reaction chamber after compressing tablet process, the air in abstraction reaction chamber is re-filled with high pure nitrogen, igniting until
Reaction terminates that product is made；
(4) product obtained in step (3) is ground, is sintered blocking, acquisition carbon solid solution nitriding silicon materials.
Further, the mass ratio of silicon powder in step (1), beta-silicon nitride powder, carbon black and ammonium chloride be 37 ~ 41:51 ~
57:5~10:2。
Further, the revolving speed of ball milling described in step (1) is 200 ~ 300rpm, and the time of ball milling is 20 ~ 30 hours.
Further, the temperature of infrared drying oven described in step (2) is 80 ~ 100 degrees Celsius.
Further, addition Al described in step (2)2O3And Y2O3Quality be that the total matter of substance is added in step (1)
The 3 ~ 5% of amount
Further, it is 7.5 megapascal that pressure in reaction chamber is filled with after high pure nitrogen in step (3).
Further, sintering condition described in step (4) is 700 ~ 900 degrees Celsius, under 35 ~ 40 megapascal air pressures.
The present invention also provides carbon solid solution nitriding silicon materials made from the preparation method described according to the above technical scheme.
Compared with prior art, the medicine have the advantages that carbon solid solution nitriding silicon materials prepared by the present invention pass through machinery
Alloying and self-propagating reaction method are dissolved carbon in silicon nitride to regulate and control the chemical bond in silicon nitride, the carbon solid solution nitriding of preparation
Silicon materials are covalent bond and metallic bond mixed type, are avoided due to silicon nitride/silicon carbide fiber circle in traditional material microstructure
Performance degradation caused by face achievees the purpose that the mechanical performance and wear-resisting property of strengthening silicon nitride ceramic material.Compared to carbon
SiClx fiber reinforcement silicon nitride, the carbon solid solution nitriding silicon obtained based on preparation method of the present invention is it is possible to prevente effectively from by phase boundary and crystalline substance
Boundary excuse me, but I must be leaving now the rudiment and extension of caused micro-crack, improve the performance of material and the safety and reliability of military service.System of the present invention
Standby carbon solid solution nitriding silicon, fracture toughness reach 10.4MPam0.5, it is 2 times of left sides of the silicon nitride ceramics of prior art production
The right side, wear rate are the 1/2 of pure silicon nitride, and carbon solid solution nitriding silicon materials of the present invention have crystallinity height, high fracture tough
Property resists the advantages that wear-resisting, lightweight；In high speed ceramic bearing, the fields such as anticorrosive ceramic coating have a wide range of applications；And it makes
Standby simple process is reliable and stable, low to process conditions susceptibility, is conducive to industrial promote and prepares.
Detailed description of the invention
Fig. 1 is density of electronic states distribution map；Wherein, figure (a) is the electronic state of the pure silicon nitride material prepared in embodiment 1
Density profile, figure (b) are the density of electronic states distributions of the carbon solid solution nitriding silicon materials of the solid solution carbon 10% prepared in embodiment 3
Figure；
Fig. 2 is the XRD diagram of the carbon solid solution nitriding silicon phase structure of embodiment 1-3 preparation；
Fig. 3 is the pattern and constituent analysis figure of carbon solid solution nitriding silicon prepared by embodiment 2；Wherein, figure (a) is scanning electron microscope photograph
Piece, figure (b) are the distribution map of nitrogen, and figure (c) is the distribution map of carbon, and figure (d) is the distribution map of element silicon；
Fig. 4 is to be dissolved carbon (content) to the analysis chart of silicon nitride material density；
Fig. 5 is the vickers indentation figure of carbon solid solution nitriding silicon；Wherein, figure (a) is 1 gained pure silicon nitride of embodiment, and figure (b) is to implement
The carbon solid solution nitriding silicon of carbon 5% is dissolved obtained by example 2, figure (c) is the carbon solid solution nitriding silicon that carbon 10% is dissolved obtained by embodiment 3；
The hardness and fracture toughness that Fig. 6 is carbon solid solution nitriding silicon obtained by embodiment 1-3 are with the variation relation figure for being dissolved concentration of carbon；
Fig. 7 is the abrasion resistance figure of carbon solid solution nitriding silicon obtained by embodiment 1-4.
Specific embodiment
In order to which those skilled in the art better understood when technical solution provided by the present invention, below with reference to specific
Embodiment is illustrated.
Embodiment 1
Silicon powder 41g, beta-silicon nitride powder 57g are weighed respectively and ammonium chloride 2g is uniformly mixed, and are added after being placed in mechanical ball grinding jar suitable
The ethyl alcohol of amount, seals to extract in tank after ball grinder and is filled with nitrogen after air, in comprehensive planetary high-energy ball mill with
The speed ball milling of 250rpm 24 hours；After mechanical ball mill in infrared drying oven 80 degrees Celsius drying 24 hours, with 3% mass ratio
Al2O3The Y of powder and 3% mass ratio2O3Powder mixing, Mechanical pressing；The piece merging self-propagating reaction pressed is intracavitary, it extracts
Air in reaction chamber is re-filled with high pure nitrogen until air pressure reaches 7.5 megapascal, and igniting is until reaction terminates；It will after reaction
The intracavitary product of self-propagating reaction grind, under the air pressure of 700 degree Celsius of 35 megapascal use discharge plasma sintering handle
The product sinters that self-propagating reaction is obtained are blocking, obtain pure silicon nitride material.
Embodiment 2
It weighs silicon powder 39g, beta-silicon nitride powder 54g, carbon black 5g and ammonium chloride 2g respectively to be uniformly mixed, after being placed in mechanical ball grinding jar
Suitable ethyl alcohol is added, is extracted in tank after sealing ball grinder and is filled with nitrogen after air, then in comprehensive planetary milling
With the speed ball milling of 200rpm 20 hours in machine；After mechanical ball mill in infrared drying oven 80 degrees Celsius drying 24 hours, with 3%
The Al of mass ratio2O3The Y of powder and 4% mass ratio2O3Powder mixing, Mechanical pressing；The piece pressed is placed in self-propagating reaction chamber
Interior, the air in abstraction reaction chamber is re-filled with high pure nitrogen until air pressure reaches 7.5 megapascal.Then igniting is until reaction terminates；
The intracavitary product of self-propagating reaction is ground, and is then burnt under the air pressure of 800 degree Celsius of 40 megapascal with plasma discharging
The product sinters that knot obtains self-propagating reaction are blocking, obtain the carbon solid solution nitriding silicon of solid solution carbon 5%.It is measured, 5% obtained
The density of carbon solid solution nitriding silicon materials is 3.38g/cm3, hardness 1260HV10, fracture toughness 10.4MPam0.5。
Embodiment 3
Silicon powder 37g, beta-silicon nitride powder 51g, carbon black 10g and ammonium chloride 2g are weighed respectively to be uniformly mixed, and are placed in mechanical ball grinding jar
After be added suitable ethyl alcohol, seal to extract in tank after ball grinder and be filled with nitrogen after air, then in comprehensive planetary high energy ball
With the speed ball milling of 300rpm 30 hours in grinding machine；After mechanical ball mill in infrared drying oven 100 degrees Celsius drying 24 hours, with
The Al of 5% mass ratio2O3The Y of powder and 5% mass ratio2O3Powder mixing, Mechanical pressing；The piece pressed is placed in self-propagating reaction
Intracavitary, the air in abstraction reaction chamber is re-filled with high pure nitrogen until air pressure reaches 7.5 megapascal, and igniting is until reaction terminates；It will
The intracavitary product of self-propagating reaction after reaction is ground, and is then used and is put under the air pressure of 900 degree Celsius of 40 megapascal
The product sinters that electric plasma agglomeration obtains self-propagating reaction are blocking, obtain the carbon solid solution nitriding silicon of solid solution carbon 10%.It obtains
The density of 10% carbon solid solution nitriding silicon materials is 3.37g/cm3, hardness 1330HV10, fracture toughness 10.1MPam0.5。
By the carbon solid solution nitriding silicon materials of the pure silicon nitride material prepared in embodiment 1 and the solid solution carbon 10% of above-mentioned preparation
Density of electronic states distribution compare and analyze, as shown in Figure 1, the dotted line in figure is fermi level, by Fig. 1 (a) as it can be seen that Fermi
Energy level is located at the top of valence band, shows that chemical bond belongs to covalent key type in silicon nitride material, by Fig. 1 (b) as it can be seen that fermi level
It is moved down to the middle position of valence band from the top of valence band, shows that chemical bond belongs to covalent bond and metallic bond in carbon solid solution nitriding silicon
Mixed type, it is confirmed that, having after carbon solid solution on silicon nitride chemical bond influences.
Object phase point is carried out to the carbon solid solution nitriding silicon obtained with Philip X-ray diffractometer (X'pertpowderXRD)
Analysis, Fig. 2 are the XRD diagram of the carbon solid solution nitriding silicon phase structure of embodiment 1-3 preparation；As shown in Fig. 2, containing in solid solution carbon mass ratio
When amount is lower than 10%, material has the hexagonal structure of silicon nitride, when solid solution carbon quality is higher than 10% than content, cubic silicon carbide
Silicon is mutually precipitated from hexagonal phase, and surface is dissolved the solubility of carbon in silicon nitride in 10% mass ratio or so.
Pattern and ingredient are carried out to prepared carbon solid solution nitriding silicon materials with NovaNano450 field emission scanning electron microscope
Analysis, Fig. 3 are the pattern and constituent analysis figure of carbon solid solution nitriding silicon prepared by embodiment 2；Wherein, figure (a) is scanning electron microscope photograph
Piece, figure (b) are the distribution map of nitrogen, and figure (c) is the distribution map of carbon, and figure (d) is the distribution map of element silicon；Such as Fig. 3 institute
Show, three kinds of nitrogen, carbon, silicon elements are uniformly distributed formation carbon solid solution nitriding silicon in the sample.
Characterization point is carried out to the density of carbon solid solution nitriding silicon with the gentle drainage in day [solid body densitometer ET-320] is weighed
Analysis, Fig. 4 are solid solutions carbon (content) to silicon nitride material density analysis figure；As shown in figure 4, with the increase of solid solution concentration of carbon, nitrogen
The density of silicon nitride material reduces, it is seen then that carbon is dissolved the density that can reduce silicon nitride material.
It is characterized with indentation crack, hardness and fracture toughness of the impression instrument to the carbon solid solution nitriding silicon of preparation, Fig. 5 is
The vickers indentation figure of carbon solid solution nitriding silicon；Wherein, figure (a) is 1 gained pure silicon nitride of embodiment, and figure (b) is solid obtained by embodiment 2
The carbon solid solution nitriding silicon of molten carbon 5%, figure (c) are the carbon solid solution nitriding silicon that carbon 10% is dissolved obtained by embodiment 3；As seen from Figure 5, solid
The crack length of the carbon solid solution nitriding Gui Zhong impression corner of molten carbon 5% is most short, this illustrates that the fracture toughness of sample at this time is best.
The hardness and fracture toughness that Fig. 6 is carbon solid solution nitriding silicon obtained by embodiment 1-3 are with the variation relation figure for being dissolved concentration of carbon；By Fig. 6
As it can be seen that the hardness of silicon nitride material rises after falling before, and the fracture toughness of silicon nitride material with the increase of solid solution concentration of carbon
Then first rise and declines afterwards.It is found that the mechanical property of silicon nitride material can be regulated and controled by the concentration of regulation solid solution carbon.
Embodiment 4
Silicon powder 35g, beta-silicon nitride powder 48g, carbon black 15g and ammonium chloride 2g are weighed respectively to be uniformly mixed, and are placed in mechanical ball grinding jar
After be added suitable ethyl alcohol, seal to extract in tank after ball grinder and be filled with nitrogen after air, then in comprehensive planetary high energy ball
With the speed ball milling of 250rpm 25 hours in grinding machine；
After mechanical ball mill in infrared drying oven 90 degrees Celsius drying 26 hours, the Al with 4% mass ratio2O3Powder and 5% mass
The Y of ratio2O3Powder mixing, Mechanical pressing；The piece merging self-propagating reaction pressed is intracavitary, and the air in abstraction reaction chamber fills again
Enter high pure nitrogen until air pressure reaches 7.5 megapascal, igniting is until reaction terminates；By the intracavitary life of self-propagating reaction after reaction
It grinds at object, then self-propagating reaction is obtained with discharge plasma sintering under the air pressure of 800 degree Celsius of 40 megapascal
Product sinters it is blocking, obtain solid solution carbon 15% carbon solid solution nitriding silicon.
The abrasion resistance of carbon solid solution nitriding silicon is characterized with pin disk friction wear testing machine (RTEC MFT-500),
Fig. 7 is the abrasion resistance figure of carbon solid solution nitriding silicon；Frrction load is 100 Ns, and the testing time 15 minutes, friction rate was 6 millimeters
It is per second；As seen from Figure 7, the wear rate of carbon solid solution nitriding silicon decreases compared to the pure silicon nitride not containing solid solution carbon, with
Carbon solid solution concentration increase wear rate fall before after rise, be dissolved concentration of carbon be 5%-10% quality ratio when abrasion resistance most
It is excellent.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (8)
1. a kind of preparation method of carbon solid solution nitriding silicon materials, comprising the following steps:
(1) silicon powder, beta-silicon nitride powder, carbon black and ammonium chloride are uniformly mixed and are placed in ball grinder, it is close after addition dehydrated alcohol
Blocking grinding jar extracts after the air in tank is filled with high-purity inert nitrogen and carries out ball milling；
(2) dry in infrared drying oven after ball milling, Al is added in the powder after drying2O3And Y2O3Compressing tablet process after mixing；
(3) be placed in self-propagating reaction chamber after compressing tablet process, the air in abstraction reaction chamber is re-filled with high pure nitrogen, igniting until
Reaction terminates that product is made；
(4) product obtained in step (3) is ground, is sintered blocking, acquisition carbon solid solution nitriding silicon materials.
2. the preparation method of carbon solid solution nitriding silicon materials according to claim 1, which is characterized in that silicon powder, β-in step (1)
The mass ratio of silicon nitride powder, carbon black and ammonium chloride is 35 ~ 41:48 ~ 57:5 ~ 10:2.
3. the preparation method of carbon solid solution nitriding silicon materials according to claim 1, which is characterized in that ball described in step (1)
The revolving speed of mill is 200 ~ 300rpm, and the time of ball milling is 20 ~ 30 hours.
4. the preparation method of carbon solid solution nitriding silicon materials according to claim 1, which is characterized in that red described in step (2)
The temperature of outer drying box is 80 ~ 100 degrees Celsius.
5. the preparation method of carbon solid solution nitriding silicon materials according to claim 1, which is characterized in that described in step (2)
Al is added2O3And Y2O3Quality be that the 3 ~ 5% of substance gross mass is added in step (1).
6. the preparation method of carbon solid solution nitriding silicon materials according to claim 1, which is characterized in that step is filled with height in (3)
Pressure is 7.5 megapascal in reaction chamber after pure nitrogen gas.
7. the preparation method of carbon solid solution nitriding silicon materials according to claim 1, which is characterized in that burnt described in step (4)
Knot condition is 700 ~ 900 degrees Celsius, under 35 ~ 40 megapascal air pressures.
8. carbon solid solution nitriding silicon materials made from preparation method as claimed in any one of claims 1 to 7.
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| CN112159236A (en) * | 2020-10-19 | 2021-01-01 | 江苏贝色新材料有限公司 | High-thermal-conductivity silicon nitride ceramic substrate and preparation method thereof |
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