CN109400174A - A kind of preparation method nitrogenizing silicon substrate high temperature antiwear and antifriction composite material - Google Patents
A kind of preparation method nitrogenizing silicon substrate high temperature antiwear and antifriction composite material Download PDFInfo
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- CN109400174A CN109400174A CN201811332482.5A CN201811332482A CN109400174A CN 109400174 A CN109400174 A CN 109400174A CN 201811332482 A CN201811332482 A CN 201811332482A CN 109400174 A CN109400174 A CN 109400174A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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Abstract
The present invention relates to a kind of preparation methods for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material, method includes the following steps: (1) by α-Si3N4And Ti3SiC2It is added in ball mill, it is mixed up to mixed-powder through wet type ball;(2) it is fitted into graphite jig after the mixed-powder drying and screening and carries out precompressed, obtains pre- pressure-like;(3) for the pre- pressure-like after high temperature and pressure is sintered, furnace cooling obtains blank;(4) the blank is after surface polishing treatment to get nitride silicon based composite material.Preparation process of the present invention simple controllable, high production efficiency, powder are not necessarily to specially treated, are suitable for batch production.Gained finished product high temperature antiwear and antifriction excellent effect, substantially prolongs the service life of ceramic component in the high temperature environment.
Description
Technical field
The present invention relates to new material technology field more particularly to a kind of systems for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material
Preparation Method.
Background technique
In recent years, with the development in the fields such as aerospace, Shipping and defense military, to structural ceramics tribology
The requirement of performance is more and more harsher, if material itself cannot achieve self-lubricating or high wear-resistant, this can greatly shorten mechanical
The service life of component is all a kind of huge waste for manpower and material resources.In numerous ceramic materials, silicon nitride due to
Its high mechanical strength, good thermal shock resistance, corrosion-resistant, the anti-oxidant and characteristics such as environmental-friendly, to be processed to axis
It holds, the components such as valve, sealing element, radar irdome and guided missile tail nozzle play an important role.
However, the maintenance for ceramic performance, high temperature is an extremely disadvantageous factor.The effect of thermal stress can seriously
The mechanical property for deteriorating ceramics, to reduce the tribological property of material.Some researches show that when test temperature is more than
At 600 DEG C, the coefficient of friction of silicon nitride is maintained between 0.8 ~ 1, wear rate 10-3 mm3/Nm~10-2mm3/ Nm, so poor profit
Sliding and abrasion is to be unable to satisfy the actual demand of industry.Therefore need one kind has antiwear and friction reduction property suitable for hot environment
Silicon nitride material.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of simple controllable, high production efficiency nitridation silicon substrate high temperature is anti-
Grind the preparation method of Antifriction Composites.
To solve the above problems, a kind of preparation side for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material of the present invention
Method, comprising the following steps:
(1) by mass percentage, by 10 ~ 30% α-Si3N4With 70 ~ 90% Ti3SiC2It is added in ball mill, it is mixed through wet type ball
Up to mixed-powder;
(2) it is fitted into graphite jig after the mixed-powder drying and screening and carries out precompressed, obtains pre- pressure-like;
(3) for the pre- pressure-like after high temperature and pressure is sintered, furnace cooling obtains blank;
(4) the blank is after surface polishing treatment to get nitride silicon based composite material.
The step (1) in α-Si3N4Granularity be 0.5 ~ 1.5 μm, purity be greater than 99%.
The step (1) in Ti3SiC2Granularity less than 5 μm, purity be greater than 99%.
The step (1) in ball mill grinding jar be polytetrafluoroethylene (PTFE) ball grinder, abrading-ball is silicon nitride ball.
(1) middle ball milling condition refers to that ratio of grinding media to material is 8 ~ 10:1 to the step, and revolving speed is 200 ~ 300r/min, Ball-milling Time 8
~12h。
(2) middle prefabricating condition is finger pressure for 80MPa to the step, and the dwell time is 10 ~ 15s.
(3) high temperature pressure sintering conditions are finger pressure for 30 ~ 40MPa to the step, and sintering temperature is 1650 ~ 1700 DEG C,
Heating rate is 100 DEG C/min, and soaking time is 8 ~ 10min, vacuum degree 10-2~10-1Pa。
Compared with the prior art, the present invention has the following advantages:
1, the present invention chooses Ti3SiC2It in situ generated micro- for persursor material using its pyrolytic and the characteristic of nitridation
The TiC of metrical scale (1 ~ 2 μm)0.3N0.7Particle can be evenly dispersed in block materials (referring to Fig. 1), solve letter
The problem that material caused by Single Mechanical stirs is reunited, to realize the improvement of high-temperature behavior;Meanwhile under the high temperature conditions, TiO2
Oxidation film can be formed, it plays the wear-resistant effect of high-temperature antifriction (referring to fig. 2) as one layer of protection.
2, nitride silicon based composite material prepared by the present invention carries out friction mill using HT-1000 high temperature friction and wear testing machine
Damage test: antithesis ball is Si3N4Ceramic Balls, load are 10 N, and sliding linear velocity is 0.13 m/s, and friction radius is 3 mm, stroke
For 234 m, test temperature is respectively 25 DEG C, 300 DEG C, 600 DEG C and 900 DEG C;Coefficient of friction and wear rate are that 3 tests are average
Value.The results show that nitride silicon based composite material prepared by the present invention have good mechanical performance and tribological property (referring to
Fig. 3 ~ 4).When test temperature is 900 DEG C, 11 ~ 11.5GPa of surface hardness, 5.0 ~ 5.2MPam of fracture toughness1/2, friction
Coefficient is 0.40 ~ 0.45, and wear rate is less than or equal to 6.5 × 10-6 mm3/Nm。
3, preparation process of the present invention simple controllable, high production efficiency, powder is not necessarily to specially treated, is suitable for batch production.
Gained finished product high temperature antiwear and antifriction excellent effect, substantially prolongs the service life of ceramic component in the high temperature environment.
4, the present invention can provide a kind of new thinking for the preparation and optimization of multiphase composite.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is the stereoscan photograph of silicon nitride composite material of the present invention.
Fig. 2 is stereoscan photograph of the silicon nitride composite material of the present invention at 900 DEG C.
Fig. 3 is the variation diagram of silicon nitride composite material coefficient of friction at different temperatures in the embodiment of the present invention 1 ~ 3.
Fig. 4 is the variation diagram of silicon nitride composite material wear rate at different temperatures in the embodiment of the present invention 1 ~ 3.
Specific embodiment
A kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material of embodiment 1, comprising the following steps:
(1) by mass percentage, by 10% α-Si3N4With 90% Ti3SiC2It is added in planetary ball mill, is in ratio of grinding media to material
It is mixed to get mixed-powder that wet type ball is carried out under conditions of 10:1, revolving speed are 300 r/min, Ball-milling Time is 10 h.
(2) it is pressure 80MPa in 25 mm cylindrical graphite molds, pressure maintaining that diameter is fitted into after mixed-powder drying and screening
Precompressed is carried out under conditions of time 10s, obtains pre- pressure-like.
(3) pre- pressure-like carries out high temperature and pressure sintering, and high temperature and pressure sintering condition is that finger pressure is 30MPa, and sintering temperature is
1680 DEG C, heating rate is 100 DEG C/min, soaking time 10min, vacuum degree 10-2Pa.Then room temperature is cooled to the furnace,
Obtain blank.
(4) blank is after surface polishing treatment to get nitride silicon based composite material.
Use the hardness of dimension formula high-temperature hardness gauge test material, test condition are as follows: loaded load 10kg, duration 10s.
Pure Si3N4And Si3N4Hardness difference of the based composites at 25 DEG C, 300 DEG C, 600 DEG C and 900 DEG C is as shown in table 1.
Table 1: pure Si3N4And Si3N4Vickers hardness of the based composites at 25 DEG C, 300 DEG C, 600 DEG C and 900 DEG C
A kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material of embodiment 2, comprising the following steps:
(1) by mass percentage, by 20% α-Si3N4With 80% Ti3SiC2It is added in planetary ball mill, is in ratio of grinding media to material
It is mixed to get mixed-powder that wet type ball is carried out under conditions of 10:1, revolving speed are 300 r/min, Ball-milling Time is 10 h.
(2) it is pressure 80MPa in 25 mm cylindrical graphite molds, pressure maintaining that diameter is fitted into after mixed-powder drying and screening
Precompressed is carried out under conditions of time 10s, obtains pre- pressure-like.
(3) pre- pressure-like carries out high temperature and pressure sintering, and high temperature and pressure sintering condition is that finger pressure is 30MPa, and sintering temperature is
1680 DEG C, heating rate is 100 DEG C/min, soaking time 10min, vacuum degree 10-2Pa.Then room temperature is cooled to the furnace,
Obtain blank.
(4) blank is after surface polishing treatment to get nitride silicon based composite material.
A kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material of embodiment 3, comprising the following steps:
(1) by mass percentage, by 30% α-Si3N4With 70% Ti3SiC2It is added in planetary ball mill, is in ratio of grinding media to material
It is mixed to get mixed-powder that wet type ball is carried out under conditions of 10:1, revolving speed are 300 r/min, Ball-milling Time is 10 h.
(2) it is pressure 80MPa in 25 mm cylindrical graphite molds, pressure maintaining that diameter is fitted into after mixed-powder drying and screening
Precompressed is carried out under conditions of time 10s, obtains pre- pressure-like.
(3) pre- pressure-like carries out high temperature and pressure sintering, and high temperature and pressure sintering condition is that finger pressure is 30MPa, and sintering temperature is
1680 DEG C, heating rate is 100 DEG C/min, soaking time 10min, vacuum degree 10-2Pa.Then room temperature is cooled to the furnace,
Obtain blank.
(4) blank is after surface polishing treatment to get nitride silicon based composite material.
The fracture toughness of material is calculated using indentation method.Experiment is at least repeated 10 times and then is averaged every time.It is pure
Si3N4And Si3N4Fracture toughness difference of the based composites at 25 DEG C, 300 DEG C, 600 DEG C and 900 DEG C is as shown in table 2.
The pure Si of table 23N4And Si3N4Fracture toughness of the based composites at 25 DEG C, 300 DEG C, 600 DEG C and 900 DEG C
A kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material of embodiment 4, comprising the following steps:
(1) by mass percentage, by 15% α-Si3N4With 85% Ti3SiC2It is added in planetary ball mill, is in ratio of grinding media to material
It is mixed to get mixed-powder that wet type ball is carried out under conditions of 8:1, revolving speed are 200 r/min, Ball-milling Time is 12 h.
(2) it is pressure 80MPa in 25 mm cylindrical graphite molds, pressure maintaining that diameter is fitted into after mixed-powder drying and screening
Precompressed is carried out under conditions of time 15s, obtains pre- pressure-like.
(3) pre- pressure-like carries out high temperature and pressure sintering, and high temperature and pressure sintering condition is that finger pressure is 40MPa, and sintering temperature is
1650 DEG C, heating rate is 100 DEG C/min, soaking time 9min, vacuum degree 10-1Pa.Then it cools to room temperature with the furnace, obtains
To blank.
(4) blank is after surface polishing treatment to get nitride silicon based composite material.
A kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material of embodiment 5, comprising the following steps:
(1) by mass percentage, by 25% α-Si3N4With 75% Ti3SiC2It is added in planetary ball mill, is in ratio of grinding media to material
It is mixed to get mixed-powder that wet type ball is carried out under conditions of 9:1, revolving speed are 250 r/min, Ball-milling Time is 8 h.
(2) it is pressure 80MPa in 25 mm cylindrical graphite molds, pressure maintaining that diameter is fitted into after mixed-powder drying and screening
Precompressed is carried out under conditions of time 12s, obtains pre- pressure-like.
(3) pre- pressure-like carries out high temperature and pressure sintering, and high temperature and pressure sintering condition is that finger pressure is 35MPa, and sintering temperature is
1700 DEG C, heating rate is 100 DEG C/min, and soaking time 8min, vacuum degree is 5 × 10-2Pa.Then room is cooled to the furnace
Temperature obtains blank.
(4) blank is after surface polishing treatment to get nitride silicon based composite material.
In above-described embodiment 1 ~ 5, α-Si3N4Granularity be 0.5 ~ 1.5 μm, purity be greater than 99%.Ti3SiC2Granularity be less than
5 μm, purity is greater than 99%.The grinding jar of ball mill is polytetrafluoroethylene (PTFE) ball grinder, and abrading-ball is silicon nitride ball.
Claims (7)
1. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material, comprising the following steps:
(1) by mass percentage, by 10 ~ 30% α-Si3N4With 70 ~ 90% Ti3SiC2It is added in ball mill, it is mixed through wet type ball
Up to mixed-powder;
(2) it is fitted into graphite jig after the mixed-powder drying and screening and carries out precompressed, obtains pre- pressure-like;
(3) for the pre- pressure-like after high temperature and pressure is sintered, furnace cooling obtains blank;
(4) the blank is after surface polishing treatment to get nitride silicon based composite material.
2. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material as claimed in claim 1, it is characterised in that: described
Step (1) in α-Si3N4Granularity be 0.5 ~ 1.5 μm, purity be greater than 99%.
3. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material as claimed in claim 1, it is characterised in that: described
Step (1) in Ti3SiC2Granularity less than 5 μm, purity be greater than 99%.
4. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material as claimed in claim 1, it is characterised in that: described
Step (1) in ball mill grinding jar be polytetrafluoroethylene (PTFE) ball grinder, abrading-ball is silicon nitride ball.
5. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material as claimed in claim 1, it is characterised in that: described
(1) middle ball milling condition refers to that ratio of grinding media to material is 8 ~ 10:1 to step, and revolving speed is 200 ~ 300r/min, and Ball-milling Time is 8 ~ 12h.
6. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material as claimed in claim 1, it is characterised in that: described
(2) middle prefabricating condition is finger pressure for 80MPa to step, and the dwell time is 10 ~ 15s.
7. a kind of preparation method for nitrogenizing silicon substrate high temperature antiwear and antifriction composite material as claimed in claim 1, it is characterised in that: described
(3) high temperature pressure sintering conditions are finger pressure for 30 ~ 40MPa to step, and sintering temperature is 1650 ~ 1700 DEG C, and heating rate is
100 DEG C/min, soaking time is 8 ~ 10min, vacuum degree 10-2~10-1Pa。
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Cited By (1)
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CN110759737A (en) * | 2019-11-19 | 2020-02-07 | 中国科学院兰州化学物理研究所 | Preparation method of high-performance silicon nitride-based composite ceramic |
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