CN106518124B - A kind of carbon fiber/sialon ceramic composite material and preparation method and application - Google Patents
A kind of carbon fiber/sialon ceramic composite material and preparation method and application Download PDFInfo
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- CN106518124B CN106518124B CN201611025470.9A CN201611025470A CN106518124B CN 106518124 B CN106518124 B CN 106518124B CN 201611025470 A CN201611025470 A CN 201611025470A CN 106518124 B CN106518124 B CN 106518124B
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- sialon
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 88
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 88
- 239000000919 ceramic Substances 0.000 title claims abstract description 82
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 238000003466 welding Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000004381 surface treatment Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 230000008021 deposition Effects 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 229910052593 corundum Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 8
- 229910017083 AlN Inorganic materials 0.000 claims description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 238000004080 punching Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 230000016507 interphase Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 150000001721 carbon Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- C04B35/597—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 oxynitride, e.g. SIALONS
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The present invention relates to ceramic composite technical field, a kind of carbon fiber/sialon ceramic composite material and preparation method and application are disclosed.Invention introduces modified carbon fibers to be added in Sialon ceramics, solve the problems, such as that Sialon ceramic material performance is insufficient in the prior art, by to surface treatment of carbon fibers, it solves the problems, such as carbon fiber and Sialon ceramics pyroreaction and its interphase match, has obtained a kind of low cost and high performance carbon fiber/sialon ceramic composite material.The present invention prepares friction welding (FW) stirring-head as raw material using carbon fiber/sialon ceramic composite material, carbon fiber/sialon ceramic composite material has preferable toughness, very high hardness and wearability, and very high high-temperature oxidation resistance, the carbon fiber that the present invention is prepared/sialon ceramic composite material stirring-head high temperature resistant (1000 DEG C or more), intensity and toughness are high, wearability is good, long service life, and preparation process of the invention is at low cost, preparation process is simple, parameter is controllable.
Description
Technical field
The present invention relates to ceramic composite technical fields, more particularly, to a kind of carbon fiber/Sialon ceramics composite wood
Material and preparation method and application.
Background technique
Sialon ceramics have at high temperature hardness height, good toughness, creep is small, anti-thermal shock inoxidizability is strong, the coefficient of expansion is small,
The superior physical and chemical performances such as chemical stability is high, wear-resistant, corrosion-resistant.And its process is mature controllably, raw material is domestic
Change degree height, relative inexpensiveness.Therefore, Sialon ceramics is currently to substitute existing high temperature resistant stirring head material, prepares high-performance
The most ideal material system of inexpensive stirring friction welding agitator head.But the Sialon ceramics stirring-head deficiency big there are still brittleness, this
Its popularization and application is seriously limited, there is an urgent need to improve its toughness.Carbon fiber is low with density, intensity and modulus is high, high-temperature stable
It the advantages that good, no creep of property, endurance and good corrosion resistance, is now widely used in ceramic matric composite, numerous studies
Show that the comprehensive performances such as intensity and the toughness of ceramic material can be significantly improved.
The fast development of current high performance ship depends not only on the high-intensitive new diseases such as aluminium alloy, also relies on
The progress of its welding technique.But there are two kinds of different-metal material welding problems of aluminum steel, agitating frictions to weld conduct for high speed Aluminium ships
A kind of novel solid phase connecting method, it is not substantially by factors such as material physical chemistry performance, mechanical performance and crystal structures
It influences, there is great advantage for the welding of dissimilar material.Therefore, agitating friction weldering is to solve current high-speed ship aluminum steel weldering
Connect the preferred interconnection technique of problem.
" heart " that stirring-head is welded as agitating friction, material and structure are the cores of agitating friction welding technology.Stirring
The heat that head directly bears welding process carries, power carries and fretting wear, therefore it is required that the material for being used to manufacture stirring-head need to have height
In the fusing point of materials to be welded, intensity, hardness and toughness, good antiwear property and heat-resisting quantity etc..Aluminum steel is welded, by
Yu Gangwei materials with high melting point, in welding, maximum temperature is up to 1000 DEG C or more.Current common stirring head material is mainly tungsten
Sill and cubic boron nitride.But tungsten is expensive, and tungsten is difficult to be machined, and hardly possible forms special-shaped size element, and stirs
Head is polymorphic structure, therefore tungsten-bast alloy stirring-head manufacturing cost is very high.Cube BN stirring-head high-temperature stability and wearability
Good, elevated temperature strength and hardness are high, but manufacture a cube BN and need high temperature and pressure, and it is also more difficult to form special-shaped size element.Because of thirty years of age
Square BN stirring-head manufacturing cost is also very high, expensive.Therefore, urgent need Development of Novel high-performance high temperature resistant agitating friction welds
Stir head material and its low cost, controllable preparation technology.
Summary of the invention
The technical problem to be solved by the present invention is to the material property for existing Sialon ceramics is insufficient, provide it is a kind of it is low at
Originally, high-performance carbon fibre/sialon ceramic composite material preparation method.
The present invention also provides a kind of carbon fiber/Sialon ceramics stirring friction welding agitator head preparation methods.
Above-mentioned purpose of the invention is solved by following technical method:
A kind of preparation method of carbon fiber/sialon ceramic composite material is provided, comprising the following steps:
S1. surface treatment of carbon fibers: being surface-treated carbon fiber, obtains the modification carbon fiber that surface has SiC coating
Dimension, then carries out chopped；
S2. raw material is prepared and is mixed: according to the molecular formula Si of Sialon ceramics4Al2O2N6It calculates and weighs weighing accordingly
Si3N4, AlN and Al2O3, Y is added2O3After obtain mixing, mixing is subjected to ball milling using dehydrated alcohol as ball-milling medium, and in ball milling
The modified carbon fiber of step S1 is added in the process, is dried after the completion of ball milling, obtained powder sealing is stand-by；
S3. green compact are suppressed: will be carried out dry pressing through powder made from step S2, and be obtained green compact；
S4. it sinter molding: green compact is made in step S3 is put into inert gas atmosphere furnace and carry out two-step method molding；
Wherein, carbon fiber surface described in S1 prepare SiC coating method the following steps are included:
S11. carbon fiber is put into chemical vapor deposition stove；
Then deposition modified-reaction is carried out as deposition gas using trichloromethyl silane, hydrogen and argon gas, obtains surface
Modified carbon fiber with SiC coating.
The processing of step S1 carbon fiber surface solves carbon fiber and asks with Sialon ceramics pyroreaction and its interphase match
Carbon fiber, is successfully added in Sialon ceramics by topic, and carbon fiber is low with density, intensity and modulus is high, high-temperature stability
Well, the advantages that no creep, endurance and good corrosion resistance, hence it is evident that it is comprehensive to improve intensity and toughness of Sialon ceramic material etc.
Can, improve its brittleness.
Molecular formula Si is used in step S24Al2O2N6Sialon ceramics reason be that low Z value is serial (Z=0.3, Z=0.6)
β-Sialon during the sintering process easily formed Y2SiAlO5N (B phase), Y2SiAlO5N (B phase) is unfavorable to the toughness of material, must be logical
It crosses control technological parameter and avoids Y2SiAlO5The generation of N (B phase), the β-Sialon of high Z value serial (Z=3,4) is during the sintering process
Easily form Si2Al3O7N and AlN polytype, it is unfavorable to the mechanical property of β-Sialon material.
Preferably, chopped length described in step S1 is 2~4mm.
Preferably, Y described in step S22O3For 3~6wt%.
Preferably, ball milling described in step S2 is further comprising the steps of:
S21. mixing, mill ball and ball-milling medium are fitted into ball grinder according to mass ratio 1:1.5:2；The mill ball choosing
With different size of corundum, the ball-milling medium selects dehydrated alcohol, and the ball grinder selects polytetrafluoroethylene (PTFE) ball grinder；
S22. the ball grinder installed sealing is put into ball milling 20~24 hours in planetary ball mill.
Preferably, step S2 drying process refers to 6~10 hours dry in 80 DEG C of baking ovens.
Preferably, dry pressing described in S3, which refers to, is placed in powder in Ф 30mm punching block, under 40MPa pressure, dry-pressing in advance at
Type.
Preferably, two-step method described in step S4 molding refer to the first step by green compact be placed on nitrogen pressure be 0.1~
2.1MPa, 1150 DEG C~1850 DEG C of temperature, heating rate is 10 DEG C/min, keeps the temperature 1 hour, second step is placed on nitrogen pressure and is
2.1~8.0MPa, 1400 DEG C~1830 DEG C of temperature, heating rate is 10 DEG C/min, keeps the temperature 1 hour.
Preferably, deposition modified-reaction described in step S12 refers to the flow-rate ratio of control trichloromethyl silane, hydrogen and argon gas
For 1:1.5~2:2~4, depositing temperature is 1000~1100 DEG C, deposition pressure is 700~1000Pa, and sedimentation time is 2~4 small
When.
Preferably, the weight that carbon fiber is added described in step S2 is 1~6wt%.
Present invention simultaneously provides application the carbon fiber/sialon ceramic composite material preparation method, be prepared it is low at
Originally, high-performance carbon fibre/sialon ceramic composite material.
A kind of preparation method of carbon fiber/Sialon ceramics stirring friction welding agitator head, the carbon fiber/Sialon ceramics is multiple
Condensation material is finished on numerically-controlled machine tool by the stirring-head contour structures and size of design, is obtained carbon fiber/Sialon ceramics
Stirring friction welding agitator head.
The present invention prepares friction welding (FW) stirring-head, the carbon fiber/Sialon ceramics as raw material using carbon fiber/Sialon ceramics
Friction welding (FW) stirring-head has preferable toughness, very high hardness and wearability and very high high-temperature oxidation resistance, Er Qiesai
Grand ceramics and the carbon fiber prices of raw materials are cheap, from a wealth of sources.
Beneficial effects of the present invention:
Invention introduces modified carbon fibers, and match is added into grand ceramics, solves Sialon ceramic material in the prior art
Problem that can be insufficient is maintaining existing Sialon ceramic material after modified carbon fiber is added compared to existing Sialon ceramic material
Toughness is also greatly improved on the basis of superior function.
Carbon fiber is low with density, intensity and modulus is high, and high-temperature stability is good, no creep, endurance and good corrosion resistance
The advantages that, the comprehensive performances such as intensity and the toughness of Sialon ceramics are improved, its brittleness is improved, the present invention passes through to carbon fiber surface
Surface treatment solves the problems, such as carbon fiber and Sialon ceramics pyroreaction and its interphase match, has obtained a kind of inexpensive, high-performance
Carbon fiber/sialon ceramic composite material.
The present invention is for the existing high temperature resistant stirring-head cost of raw material is high, preparation process is complicated, difficult processing and processing capacity
Greatly, the high problem of manufacturing cost provides a kind of work of Sialon ceramics stirring-head inexpensive, preparation process is simple, parameter is controllable
Process, prepared stirring-head have preferable toughness, very high hardness and wearability and very high high-temperature oxidation resistant
Property, and Sialon ceramics and the carbon fiber prices of raw materials are cheap, and it is from a wealth of sources.
Preparation process of the invention is simple, parameter is controllable, and is adjusted by raw material group meta design and preparation technology parameter,
Easily realize the optimization and regulation of the institutional framework and performance of stirring-head；
Carbon fiber prepared by the present invention/sialon ceramic composite material stirring-head high temperature resistant (1000 DEG C or more), intensity and tough
Property it is high, wearability is good, long service life.
Specific embodiment
Present invention be described in more detail combined with specific embodiments below.Unless stated otherwise, the embodiment of the present invention uses
Various raw materials can be obtained by regular market purchase, or be prepared according to the conventional method of this field, device therefor is real
Test commonly used equipment.Unless otherwise defined or described herein, all professional and scientific terms and art technology used herein are ripe
It is identical to practice meaning known to personnel.
Embodiment 1
The present embodiment provides a kind of preparation methods of carbon fiber/sialon ceramic composite material, comprising the following steps:
S1. carbon fiber is put into chemical vapor deposition stove；
S2. the flow-rate ratio for controlling deposition gas trichloromethyl silane, hydrogen and argon gas is 1:1.5:2, and depositing temperature is
1000 DEG C, deposition pressure 700Pa, sedimentation time be 2 hours, SiC coating is made in carbon fiber surface, be then chopped to
Length is that 2mm is spare；
S3. raw material is prepared and is mixed: according to the molecular formula Si of Sialon ceramics4Al2O2N6It calculates and weighs weighing accordingly
Si3N4, AlN and Al2O3, add 3wt%Y2O3Mixing is obtained, by mixing, different size of corundum and dehydrated alcohol according to matter
Amount is fitted into polytetrafluoroethylene (PTFE) ball grinder than 1:1.5:2, and the ball grinder installed sealing is put into ball milling 20 in planetary ball mill
Hour, it is carbon fiber made from 1wt% step S3 that weight, which is added, in half an hour before ball mill mixing is completed, and is then dried, obtains
The powder sealing arrived is stand-by；
S4. green compact are suppressed: will be to be done under 40MPa pressure in 30 ㎜ punching blocks in diameter through powder made from step S4
Preform is pressed, green compact are obtained；
S5. sinter molding: being made green compact for step S5 and be put into nitrogen atmosphere stove and carry out temperature programming, using two-step method
Molding, it is 0.1MPa that the first step, which is placed on nitrogen pressure, and temperature is 1150 DEG C, with heating rate for 10 DEG C/min, keeps the temperature 1 hour,
It is 2.1MPa that second step, which is placed on nitrogen pressure, and temperature is 1400 DEG C, with heating rate for 10 DEG C/min, keeps the temperature 1 hour.
Embodiment 2
The present embodiment provides a kind of preparation methods of carbon fiber/sialon ceramic composite material, comprising the following steps:
S1. carbon fiber is put into chemical vapor deposition stove；
S2. the flow-rate ratio for controlling deposition gas trichloromethyl silane, hydrogen and argon gas is 1:1.7:3, and depositing temperature is
1050 DEG C, deposition pressure 800Pa, sedimentation time be 3 hours, SiC coating is made in carbon fiber surface, be then chopped to
Length is that 3mm is spare；
S3. raw material is prepared and is mixed: according to the molecular formula Si of Sialon ceramics4Al2O2N6It calculates and weighs weighing accordingly
Si3N4, AlN and Al2O3, add 4wt%Y2O3After obtain mixing, by mixing, different size of corundum and dehydrated alcohol according to
Mass ratio 1:1.5:2 is fitted into polytetrafluoroethylene (PTFE) ball grinder, and the ball grinder installed sealing is put into ball milling in planetary ball mill
22 hours, it was carbon fiber made from 2wt% step S3 that weight, which is added, in half an hour before ball mill mixing is completed, and was then dried,
Obtained powder sealing is stand-by；
S4. green compact are suppressed: will be to be done under 40MPa pressure in 30 ㎜ punching blocks in diameter through powder made from step S4
Preform is pressed, green compact are obtained；
S5. sinter molding: being made green compact for step S5 and be put into nitrogen atmosphere stove and carry out temperature programming, using two-step method
Molding, it is 1MPa that the first step, which is placed on nitrogen pressure, and temperature is 1300 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 1 hour, second
It is 5.0MPa that step, which is placed on nitrogen pressure, and temperature is 1500 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 1 hour；
Embodiment 3
The present embodiment provides a kind of preparation methods of carbon fiber/sialon ceramic composite material, comprising the following steps:
S1. carbon fiber is put into chemical vapor deposition stove；
S2. the flow-rate ratio for controlling deposition gas trichloromethyl silane, hydrogen and argon gas is 1:1.9:4, and depositing temperature is
1100 DEG C, deposition pressure 900Pa, sedimentation time be 4 hours, SiC coating is made in carbon fiber surface, be then chopped to
Length is that 4mm is spare；
S3. raw material is prepared and is mixed: according to the molecular formula Si of Sialon ceramics4Al2O2N6It calculates and weighs weighing accordingly
Si3N4, AlN and Al2O3, add 6wt%Y2O3After obtain mixing, by mixing, different size of corundum and dehydrated alcohol according to
Mass ratio 1:1.5:2 is fitted into polytetrafluoroethylene (PTFE) ball grinder, and the ball grinder installed sealing is put into ball milling in planetary ball mill
24 hours, it was carbon fiber made from 4wt% step S3 that weight, which is added, in half an hour before ball mill mixing is completed, and was then dried,
Obtained powder sealing is stand-by；
S4. green compact are suppressed: will be to be done under 40MPa pressure in 30 ㎜ punching blocks in diameter through powder made from step S4
Preform is pressed, green compact are obtained；
S5. sinter molding: being made green compact for step S5 and be put into nitrogen atmosphere stove and carry out temperature programming, using two-step method
Molding, it is 2.1MPa that the first step, which is placed on nitrogen pressure, and temperature is 1400 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 1 hour, the
It is 8.0MPa that two steps, which are placed on nitrogen pressure, and temperature is 1600 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 1 hour；
Embodiment 4
The present embodiment provides a kind of preparation methods of carbon fiber/sialon ceramic composite material, comprising the following steps:
S1. carbon fiber is put into chemical vapor deposition stove；
S2. the flow-rate ratio for controlling deposition gas trichloromethyl silane, hydrogen and argon gas is 1:2:4, depositing temperature 1100
DEG C, deposition pressure 1000Pa, sedimentation time be 4 hours, SiC coating is made in carbon fiber surface, is then chopped to length
Degree is that 4mm is spare；
S3. raw material is prepared and is mixed: according to the molecular formula Si of Sialon ceramics4Al2O2N6It calculates and weighs weighing accordingly
Si3N4, AlN and Al2O3, add 6wt%Y2O3After obtain mixing, by mixing, different size of corundum and dehydrated alcohol according to
Mass ratio 1:1.5:2 is fitted into polytetrafluoroethylene (PTFE) ball grinder, and the ball grinder installed sealing is put into ball milling in planetary ball mill
24 hours, it was carbon fiber made from 6wt% step S3 that weight, which is added, in half an hour before ball mill mixing is completed, and was then dried,
Obtained powder sealing is stand-by；
S4. green compact are suppressed: will be to be done under 40MPa pressure in 30 ㎜ punching blocks in diameter through powder made from step S4
Preform is pressed, green compact are obtained；
S5. sinter molding: being made green compact for step S5 and be put into nitrogen atmosphere stove and carry out temperature programming, using two-step method
Molding, it is 2.1MPa that the first step, which is placed on nitrogen pressure, and temperature is 1850 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 1 hour, the
It is 8.0MPa that two steps, which are placed on nitrogen pressure, and temperature is 1830 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 1 hour；
Embodiment 5
The present embodiment provides a kind of carbon fiber/Sialon ceramics stirring friction welding agitator head preparation methods, including following step
It is rapid:
S1. carbon fiber/sialon ceramic composite material that Example 1 is prepared.
S2. above-mentioned material is finished, finally by the stirring-head contour structures and size of design on numerically-controlled machine tool
The Sialon ceramics friction welding (FW) stirring-head comprising carbon fiber is made.
Embodiment 6
The present embodiment provides a kind of carbon fiber/Sialon ceramics stirring friction welding agitator head preparation methods, including following step
It is rapid:
S1. carbon fiber/sialon ceramic composite material that Example 2 is prepared.
S2. above-mentioned material is finished, finally by the stirring-head contour structures and size of design on numerically-controlled machine tool
Carbon fiber/Sialon ceramics stirring friction welding agitator head is made.
Embodiment 7
The present embodiment provides a kind of carbon fiber/Sialon ceramics stirring friction welding agitator head preparation methods, including following step
It is rapid:
S1. carbon fiber/sialon ceramic composite material that Example 3 is prepared.
S2. above-mentioned material is finished, finally by the stirring-head contour structures and size of design on numerically-controlled machine tool
Carbon fiber/Sialon ceramics stirring friction welding agitator head is made.
Embodiment 8
The present embodiment provides a kind of carbon fiber/Sialon ceramics stirring friction welding agitator head preparation methods, including following step
It is rapid:
S1. carbon fiber/sialon ceramic composite material that Example 4 is prepared.
S2. above-mentioned material is finished, finally by the stirring-head contour structures and size of design on numerically-controlled machine tool
Carbon fiber/Sialon ceramics stirring friction welding agitator head is made.
Comparative example 1
This comparative example provides a kind of preparation method of Sialon ceramics stirring-head, and carbon fiber material is both added without in Sialon ceramics
Material, comprising the following steps:
S1. raw material is prepared and is mixed: according to the molecular formula Si of Sialon ceramics4Al2O2N6It calculates and weighs weighing accordingly
Si3N4, AlN and Al2O3, add 6wt%Y2O3After obtain mixing, by mixing, different size of corundum and dehydrated alcohol according to
Mass ratio 1:1.5:2 is fitted into polytetrafluoroethylene (PTFE) ball grinder, and the ball grinder installed sealing is put into ball milling in planetary ball mill
It 24 hours, is then dried, obtained powder sealing is stand-by；
S2. green compact are suppressed: will be to be done under 40MPa pressure in 30 ㎜ punching blocks in diameter through powder made from step S4
Preform is pressed, green compact are obtained；
S3. sinter molding: being made green compact for step S5 and be put into nitrogen atmosphere stove and carry out temperature programming, using two-step method
Molding, the first step be placed on nitrogen pressure be 2.1MPa, temperature be 1150 DEG C at, with heating rate be 10 DEG C/min to 1850 DEG C,
Heat preservation 1 hour, second step be placed on nitrogen pressure be 8.0MPa, temperature be 1400 DEG C at, with heating rate be 10 DEG C/min extremely
1830 DEG C, 1 hour is kept the temperature, Sialon ceramic material is obtained；
S4. by sialon material obtained by step S3 by the stirring-head contour structures and size of design, on numerically-controlled machine tool
It is finished, finally obtained Sialon ceramics stirring friction welding agitator head.
The performance test results and characterization
Performance detection is carried out to 5~embodiment of embodiment 8, the preparation gained stirring-head of comparative example 1, specifically: using A Ji
Mead method measures the density of material, and each data are at least surveyed three samples and are averaged.It is limited using Laizhou China instrument test apparatus
The hour V-10A Vickers of company's production, measures Vickers hardness, and load 1kg loads 10s, tests five points, be averaged
Value.The bending resistance test process of sample is carried out referring to " engineering ceramics bending strength test method " (GB6569-86),
It is measured on CSS-44100 electronic universal tester using three-point bending method.When bending strength is tested, specimen size is 4mm × 3mm
× 36mm (width x thickness × length), span 30mm, loading speed 0.5mm/min.The polishing of sample tension face, and require chamfering
(45°).Using the fracture toughness of Vicker indentation method measurement material, impression is produced by Laizhou Huayi Testing Instrument Co., Ltd.
Hour V-10A Vickers generates, loading speed 0.5mm/min, load 10kg, load time 10s.Specific testing result
As shown in table 1.
Material analysis is carried out to preparation gained stirring-head in 5~embodiment of embodiment 8, which is homogeneous texture, carbon fiber
Dimension is evenly distributed in Sialon ceramics, specific as shown in table 2.
The main performance index of 1 stirring-head of table
| Embodiment | Density (g/cm3) | Vickers hardness (HV) | Bending strength (Mpa) | Fracture toughness (MPam1/2) |
| Embodiment 5 | 3.15 | 1587 | 796 | 7.95 |
| Embodiment 6 | 3.15 | 1598 | 791 | 7.84 |
| Embodiment 7 | 3.17 | 1612 | 803 | 7.87 |
| Embodiment 8 | 3.16 | 1602 | 805 | 7.92 |
| Comparative example 1 | 3.21 | 1600 | 801 | 7.18 |
The main material of 2 stirring-head of table
| Embodiment | Carbon fiber content (wt%) | β-Sialon ceramics content (wt%) |
| Embodiment 5 | 1.00 | 99.00 |
| Embodiment 6 | 2.00 | 97.89 |
| Embodiment 7 | 4.00 | 95.28 |
| Embodiment 8 | 6.00 | 94.00 |
It is analyzed by 5~embodiment of embodiment 8 it is found that using carbon fiber/sialon ceramic composite material preparation stirring-head
Excellent material performance, density is lower, and hardness and strength are identical as the comparative example 1 of modified carbon fiber is not added, but toughness is much high
The toughness of modified carbon fiber is not added in comparative example 1, and the β of stirring-head-Sialon ceramics content is higher, carbon fiber and Sai Longtao
Porcelain associativity is good.
Claims (8)
1. a kind of preparation method of carbon fiber/sialon ceramic composite material, which comprises the following steps:
S1. surface treatment of carbon fibers: being surface-treated carbon fiber, obtains the modified carbon fiber that surface has SiC coating, so
After carry out it is chopped；
S2. raw material is prepared and is mixed: being calculated according to the molecular formula Si4Al2O2N6 of Sialon ceramics and is weighed weighing accordingly
Si3N4, AlN and Al2O3 obtain mixing after Y2O3 is added, mixing are carried out ball milling using dehydrated alcohol as ball-milling medium, and in ball
The modified carbon fiber of step S1 is added during mill, is dried after the completion of ball milling, obtained powder sealing is stand-by；
S3. green compact are suppressed: will be carried out dry pressing through powder made from step S2, and be obtained green compact；
S4. it sinter molding: green compact is made in step S3 is put into inert gas atmosphere furnace and carry out two-step method molding；
Wherein, carbon fiber surface described in S1 prepare SiC coating method the following steps are included:
S11. carbon fiber is put into chemical vapor deposition stove；Then using trichloromethyl silane, hydrogen and argon gas as deposition
Gas source carries out deposition modified-reaction, obtains the modified carbon fiber that surface has SiC coating；
It is 0.1~2.1MPa, temperature that the molding of two-step method described in step S4, which refers to that green compact are placed on nitrogen pressure by the first step,
1150 DEG C~1850 DEG C, heating rate is 10 DEG C/min, keeps the temperature 1 hour, and it is 2.1~8.0MPa that second step, which is placed on nitrogen pressure,
1400 DEG C~1830 DEG C of temperature, heating rate is 10 DEG C/min, keeps the temperature 1 hour；
The deposition modified-reaction refers to that the flow-rate ratio of control trichloromethyl silane, hydrogen and argon gas is 1:1.5~2:2~4, sinks
Accumulated temperature degree is 1000~1100 DEG C, deposition pressure is 700~1000Pa, and sedimentation time is 2~4 hours；
The modified carbon fiber being added in step S2 is 1~6wt%.
2. carbon fiber/sialon ceramic composite material preparation method according to claim 1, which is characterized in that step S1 institute
Stating chopped length is 2~4mm.
3. carbon fiber/sialon ceramic composite material preparation method according to claim 1, which is characterized in that step S2 institute
Stating Y2O3 is 3~6wt%.
4. carbon fiber/sialon ceramic composite material preparation method according to claim 1, which is characterized in that step S2 institute
It is further comprising the steps of to state ball milling:
S21. mixing, mill ball and ball-milling medium are fitted into ball grinder according to mass ratio 1:1.5:2；The mill ball is selected not
With the corundum of size, the ball grinder selects polytetrafluoroethylene (PTFE) ball grinder；
S22. the ball grinder installed sealing is put into ball milling 20~24 hours in planetary ball mill, before ball milling completes half an hour
Modified carbon fiber is added.
5. carbon fiber/sialon ceramic composite material preparation method according to claim 1, which is characterized in that step S2 is dry
Dry processing refers to 6~10 hours dry in 80 DEG C of baking ovens.
6. carbon fiber/sialon ceramic composite material preparation method according to claim 1, which is characterized in that step S3 institute
It states dry pressing and refers to and powder is placed in Ф 30mm punching block, under 40 MPa pressure, dry-pressing is preforming.
7. a kind of carbon fiber/sialon ceramic composite material, which is characterized in that the carbon fiber as described in claim 1 to 6 any one
Dimension/sialon ceramic composite material preparation method is prepared.
8. a kind of carbon fiber/Sialon ceramics stirring friction welding agitator head preparation method, which is characterized in that by claim 1 to 6
Carbon fiber/sialon ceramic composite material is prepared in carbon fiber/sialon ceramic composite material preparation method described in any one；
By the carbon fiber/sialon ceramic composite material by the stirring-head contour structures and size of design, essence is carried out on numerically-controlled machine tool
Processing, obtains carbon fiber/Sialon ceramics stirring friction welding agitator head.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN85107936A (en) * | 1985-10-23 | 1987-07-22 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Sai Long (Sialon)-boron nitride fibre matrix material and manufacture method thereof |
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| CN85107936A (en) * | 1985-10-23 | 1987-07-22 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Sai Long (Sialon)-boron nitride fibre matrix material and manufacture method thereof |
Non-Patent Citations (2)
| Title |
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| "BN纤维-Sialon复合材料的初步研究";顾培芷等;《硅酸盐学报》;19860930;第14卷(第3期);第369-372页 * |
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