CN107445640A - A kind of manufacture method of C/SiC novel mechanical sealing rings - Google Patents

A kind of manufacture method of C/SiC novel mechanical sealing rings Download PDF

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CN107445640A
CN107445640A CN201610910155.8A CN201610910155A CN107445640A CN 107445640 A CN107445640 A CN 107445640A CN 201610910155 A CN201610910155 A CN 201610910155A CN 107445640 A CN107445640 A CN 107445640A
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sealing ring
carbon fiber
manufacture method
prepared
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李建国
刘利霞
李佳佳
苏竞艳
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Shun County West Ditch Ding Ding New Mstar Technology Ltd
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Shun County West Ditch Ding Ding New Mstar Technology Ltd
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    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
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Abstract

The present invention relates to a kind of manufacture method of C/SiC novel mechanical sealing rings, by preparing carbon fiber precast body, porous C/SiC ceramic matrix composite material, preprocessing obtain honeycomb seal ring billet body, siliconising processing, preprocessing obtain the obtained C/SiC mechanical seal rings such as the sealing ring base substrate, SiC coatings, finishing of densification.The material has the performances such as densification, high intensity, high tenacity, high rigidity, high temperature resistant, corrosion-resistant and wearability, can make the life of sealing ring, and reduction changes number, reduces use cost, improves efficiency.Present invention process is simple, reproducible, suitable for batch production.

Description

A kind of manufacture method of C/SiC novel mechanical sealing rings
Technical field:
The present invention relates to a kind of manufacture method of mechanical seal ring, more particularly to a kind of system of C/SiC mechanical seal rings Make method.
Background technology:
With the development of engineering technology, the field such as petrochemical industry, atomic energy, ship, aerospace and machine-building is close to machinery Envelope proposes higher and higher requirement, can be in high speed, high pressure, high temperature, low temperature, deep-etching and containing harsh conditions such as solid particles Lower operating steady in a long-term.At present, in order to meet the requirement of these severe rugged environments, generally use SiC, Si3N4、Al2O3Deng pottery Porcelain seals.Although these ceramic seals can meet the requirement of these severe rugged environments, the intrinsic fragility of ceramics causes its clothes Poor reliability is used as a servant, in order to improve the use reliability of ceramic seal, it is necessary to solve the intrinsic fragility of ceramics.
In order to solve the fragility of ceramics, complex phase ceramic, fiber reinforced ceramic matric composite (CMCs) and layer are developed The three major controls such as shape ceramics.Wherein complex phase ceramic and ceramic layered toughness improve limited, and reliability is still limited.CMCs is from root Solve the brittleness problems of ceramic material in sheet, but conventional CMCs, because its consistency is not high, it can not meet that sealing will Ask, and sealing surface can not be worked into the requirement that finish is not more than 0.1 μm.Therefore, the present invention proposes that a kind of C/SiC is answered The preparation method of condensation material mechanical seal ring, ceramic material toughness can be improved, and can improves material density, and can realize Sealing surface finish is less than 0.1 μm of requirement.
The content of the invention:
The invention mainly relates to the preparation of D refraction statics carbon fiber precast body, the preparation of porous C/SiC ceramic matrix composite material, siliconising Processing, the preparation of SiC coatings etc..Technical scheme, mainly including following steps:
Step 1, the preparation of carbon fiber precast body
If 0 ° of laminated cloth of individual layer of dried layer, tire net, 90 ° of laminated cloths, tire net are circulated to the thickness for the design that is added to successively, and The carbon fiber precast body of design is prepared by relay acupuncture;Needling density is 25~30 pins/cm2, bulk density be 0.5~ 0.55g/cm3, the volume ratio of wherein tire stratum reticulare and laminated cloth layer is 1: 2~1: 5.
Step 2, the preparation of porous C/SiC ceramic matrix composite material
Using propylene or natural gas as reacting gas, PyC (pyrolysis is deposited in prefabricated carbon fiber body prepared by step 1 Carbon), depositing temperature is 930~1100 DEG C, and sedimentation time is 10~30h, in the monofilament carbon fiber surface system of carbon fiber precast body Pyrolytic carbon interface thick standby 100~150nm, then 1700~1900 DEG C of high-temperature heat treatments under argon gas or vacuum condition, are handled 1~2h of time, the carbon fiber precast body at the interface containing pyrolytic carbon is made.The carbon fiber precast body at the interface containing pyrolytic carbon is placed in chemistry Gaseous phase deposition stove, using trichloromethyl silane as reacting gas, SiC ceramic matrix, deposition temperature are deposited in prefabricated carbon fiber body Spend for 1000~1200 DEG C, sedimentation time is 400~500h, and it is 1.5~1.7g/cm to prepare density3Porous C/SiC it is compound Material.
Step 3:Preprocessing 1
Porous C/the SiC ceramic matrix composite material prepared to step 2 is machined out, and obtains sealing ring base substrate.Thickness is removed during processing Direction one side is reserved outside 0.3mm~0.5mm surplus, and remaining size is fully according to sealing ring drawing requirement.
Step 4:Siliconising is handled
The good sealing ring base substrate of step 3 preprocessing is subjected to siliconising processing, infiltration temperature in a vacuum furnace:1550~1600 DEG C, soaking time:1~2h, acquisition density are 2.1~2.4g/cm3, C/SiC sealing ring base substrate of the open porosity less than 1%.
Step 5:Preprocessing 2
Thickness direction (the namely rubbing surface of sealing ring) Even Grinding of the C/SiC sealing ring base substrates prepared to step 4 Processing, after processing, thickness is smaller 0.08~0.1mm than drawing requirement size.
Step 6:Deposit SiC coatings
The non-rubbing surface of sealing ring after step 5 is processed is protected by graphite paper, is placed in chemical vapor deposition Stove, using trichloromethyl silane as reacting gas, SiC ceramic coating, depositing temperature 1000 are deposited in the rubbing surface of sealing ring ~1200 DEG C, sedimentation time is 200~300h, the SiC coatings that obtained thickness is about 0.1~0.15mm.
Step 7:Finishing
The rubbing surface of sealing ring base substrate with SiC coatings prepared by step 6 carries out fine grinding, and is polished place Reason, reach the dimensional accuracy and surface smoothness (being not more than 0.1 μm) of drawing requirement, C/SiC mechanical seal rings are made.
Bending strength using the obtained C/SiC mechanical seal rings of the present invention is~180MPa, and fracture is hot for~12MPa m1/2Case hardness is~21GPa, surface smoothness~0.10.1 μm, has excellent mechanical property.
Main advantages of the present invention are:(1) large scale (thickness can be obtained by chemical vapor deposition method combination siliconizing treatment processes Degree is more than 10mm, and remaining size is unlimited.) compact texture C/SiC composites, base substrate is processed in porous state, drop The difficulty of processing and cost of low C/SiC components.(2) C/SiC ceramic-seal rings are corrosion-resistant, and high temperature resistant is wear-resistant, especially intensity High, good toughness, it is used as the mechanical seal ring of severe rugged environment, the life of sealing ring can be made, reduction changes number, and reduction makes With cost, efficiency is improved.(3) technique is simple, reproducible, suitable for batch production.
Embodiment:
Embodiment one:
Step 1, the preparation of carbon fiber precast body
If 0 ° of laminated cloth of individual layer of dried layer, tire net, 90 ° of laminated cloths, tire net are circulated to the thickness for the design that is added to successively, and The carbon fiber precast body of design is prepared by relay acupuncture;Needling density is 30 pins/cm2, bulk density .55g/cm3, its The volume ratio of middle tire stratum reticulare and laminated cloth layer is about 1: 3.
Step 2, the preparation of porous C/SiC ceramic matrix composite material
Using propylene or natural gas as reacting gas, PyC (pyrolysis is deposited in prefabricated carbon fiber body prepared by step 1 Carbon), depositing temperature is 1100 DEG C, sedimentation time 25h, and it is thick to prepare 130nm in the monofilament carbon fiber surface of carbon fiber precast body Pyrolytic carbon interface, then 1750 DEG C of high-temperature heat treatments under argon gas or vacuum condition, processing time 1.5h, be made and contain pyrolytic carbon The carbon fiber precast body at interface.The carbon fiber precast body at the interface containing pyrolytic carbon is placed in chemical vapor deposition stove, with trichloromethyl Silane deposits SiC ceramic matrix, depositing temperature is 1200 DEG C, and sedimentation time is as reacting gas in prefabricated carbon fiber body 450h, density is prepared as~1.7g/cm3Porous C/SiC ceramic matrix composite material.
Step 3:Preprocessing 1
Porous C/the SiC ceramic matrix composite material prepared to step 2 is machined out, and obtains sealing ring base substrate.Thickness is removed during processing Direction one side is reserved outside 0.3mm surplus, and remaining size is fully according to sealing ring drawing requirement.
Step 4:Siliconising is handled.
The good sealing ring base substrate of step 3 preprocessing is subjected to siliconising processing, infiltration temperature in a vacuum furnace:1550 DEG C, protect The warm time:2h, density is obtained as~2.2g/cm3, the C/SiC sealing ring base substrates of open porosity~1%.
Step 5:Preprocessing 2
Thickness direction (the namely rubbing surface of sealing ring) Even Grinding of the C/SiC sealing ring base substrates prepared to step 4 Processing, after processing, thickness is smaller 0.08mm than drawing requirement size.
Step 6:Deposit SiC coatings
The non-rubbing surface of sealing ring after step 5 is processed is protected by graphite paper, is placed in chemical vapor deposition Stove, using trichloromethyl silane as reacting gas, SiC ceramic coating, depositing temperature 1050 are deposited in the rubbing surface of sealing ring DEG C, sedimentation time 300h, the SiC coatings that obtained thickness is about 0.1mm.
Step 7:Finishing
The rubbing surface of sealing ring base substrate with SiC coatings prepared by step 6 carries out fine grinding, and is polished place Reason, reach the dimensional accuracy and surface smoothness of drawing requirement, C/SiC mechanical seal rings are made.
Bending strength~160Mpa of the C/SiC mechanical seal ring materials, fracture toughness~10MPam1/2, case hardness 20GPa, 0.1 μm of surface smoothness.
Embodiment two:
Step 1, the preparation of carbon fiber precast body
If 0 ° of laminated cloth of individual layer of dried layer, tire net, 90 ° of laminated cloths, tire net are circulated to the thickness for the design that is added to successively, and The carbon fiber precast body of design is prepared by relay acupuncture;Needling density is 25 pins/cm2, bulk density 0.5g/cm3, its The volume ratio of middle tire stratum reticulare and laminated cloth layer is about 1: 3.
Step 2, the preparation of porous C/SiC ceramic matrix composite material
Using propylene or natural gas as reacting gas, PyC (pyrolysis is deposited in prefabricated carbon fiber body prepared by step 1 Carbon), depositing temperature is 950 DEG C, sedimentation time 30h, and 150nm thickness is prepared in the monofilament carbon fiber surface of carbon fiber precast body Pyrolytic carbon interface, then 1800 DEG C of high-temperature heat treatments, processing time 1h, the carbon that the interface containing pyrolytic carbon is made are fine under vacuum Tie up precast body.The carbon fiber precast body at the interface containing pyrolytic carbon is placed in chemical vapor deposition stove, using trichloromethyl silane as instead Gas is answered, SiC ceramic matrix is deposited in prefabricated carbon fiber body, depositing temperature is 1100 DEG C, sedimentation time 400h, is prepared Density is~1.65g/cm3Porous C/SiC ceramic matrix composite material.
Step 3:Preprocessing 1
Porous C/the SiC ceramic matrix composite material prepared to step 2 is machined out, and obtains sealing ring base substrate.Thickness is removed during processing Direction one side is reserved outside 0.3mm surplus, and remaining size is fully according to sealing ring drawing requirement.
Step 4:Siliconising is handled.
The good sealing ring base substrate of step 3 preprocessing is subjected to siliconising processing, infiltration temperature in a vacuum furnace:1600 DEG C, protect The warm time:1h, density is obtained as~2.4g/cm3, the C/SiC sealing ring base substrates of open porosity~1%.
Step 5:Preprocessing 2
Thickness direction (the namely rubbing surface of sealing ring) Even Grinding of the C/SiC sealing ring base substrates prepared to step 4 Processing, after processing, thickness is smaller than drawing requirement size~0.1mm.
Step 6:Deposit SiC coatings
The non-rubbing surface of sealing ring after step 5 is processed is protected by graphite paper, is placed in chemical vapor deposition Stove, using trichloromethyl silane as reacting gas, SiC ceramic coating, depositing temperature 1200 are deposited in the rubbing surface of sealing ring DEG C, sedimentation time 300h, it is about~0.15mm SiC coatings that thickness, which is made,.
Step 7:Finishing
The rubbing surface of sealing ring base substrate with SiC coatings prepared by step 6 carries out fine grinding, and is polished place Reason, reach the dimensional accuracy and finish of drawing requirement, C/SiC mechanical seal rings are made.
Bending strength~180Mpa of the C/SiC mechanical seal ring materials, fracture toughness~12MPam1/2, case hardness 21GPa, 0.1 μm of surface smoothness.

Claims (6)

1. a kind of manufacture method of C/SiC novel mechanical sealing rings, this method includes following key step:
Step 1, the preparation of carbon fiber precast body
If 0 ° of laminated cloth of individual layer of dried layer, tire net, 90 ° of laminated cloths, tire net are circulated the thickness for the design that is added to, and passed through successively The carbon fiber precast body of design is prepared in relay acupuncture;Needling density is 25~30 pins/cm2, bulk density is 0.5~0.55g/ cm3, the volume ratio of wherein tire stratum reticulare and laminated cloth layer is 1: 2~1: 5;
Step 2, the preparation of porous C/SiC ceramic matrix composite material
Using propylene or natural gas as reacting gas, PyC (pyrolytic carbon) is deposited in prefabricated carbon fiber body prepared by step 1, is sunk Accumulated temperature degree is 930~1100 DEG C, and thick pyrolytic carbons circle of 100~150nm are prepared in the monofilament carbon fiber surface of carbon fiber precast body Face, then 1700~1900 DEG C of high-temperature heat treatments under argon gas or vacuum condition, the prefabricated carbon fiber at the interface containing pyrolytic carbon is made Body;The carbon fiber precast body at the interface containing pyrolytic carbon is placed in chemical vapor deposition stove, using trichloromethyl silane as reacting gas, SiC ceramic matrix is deposited in prefabricated carbon fiber body, depositing temperature is 1000~1200 DEG C, and it is 1.5~1.7g/ to prepare density cm3Porous C/SiC ceramic matrix composite material;
Step 3, preprocessing 1
Porous C/the SiC ceramic matrix composite material prepared to step 2 is machined out, and obtains sealing ring base substrate.Thickness direction is removed during processing Outside the reserved surplus of one side, remaining size is fully according to sealing ring drawing requirement;
Step 4, siliconising is handled
The good sealing ring base substrate of step 3 preprocessing is subjected to siliconising processing, infiltration temperature in a vacuum furnace:1550~1600 DEG C, Insulation, acquisition density is 2.1~2.4g/cm3, C/SiC sealing ring base substrate of the open porosity less than 1%;
Step 5, preprocessing 2
Thickness direction (the namely rubbing surface of sealing ring) Even Grinding of the C/SiC sealing ring base substrates prepared to step 4 is processed, After processing, thickness is smaller than drawing requirement size;
Step 6, SiC coatings are deposited
The non-rubbing surface of sealing ring after step 5 is processed is protected by graphite paper, is placed in chemical vapor deposition stove, with Trichloromethyl silane deposits SiC ceramic coating, depositing temperature is 1000~1200 as reacting gas in the rubbing surface of sealing ring DEG C, the SiC coatings that obtained thickness is about 0.1~0.15mm;
Step 7, finish
The rubbing surface of sealing ring base substrate with SiC coatings prepared by step 6 carries out fine grinding, and is processed by shot blasting, Reach the dimensional accuracy and surface smoothness (being not more than 0.1 μm) of drawing requirement, C/SiC mechanical seal rings are made.
2. the manufacture method of C/SiC novel mechanical sealing rings according to claim 1, it is characterised in that described in step 2 Pyrocarbon time of porous C/SiC ceramic matrix composite material be 10~30h;The high-temperature heat treatment time is 1~2h, with trichloromethyl Silane is 400~500h as the sedimentation time of reacting gas.
3. the manufacture method of C/SiC novel mechanical sealing rings according to claim 1 or 2, it is characterised in that institute in step 3 The processing thickness direction one side reserved margin stated is 0.3~0.5mm.
4. the manufacture method of the C/SiC novel mechanical sealing rings according to one of claim 1-3, it is characterised in that step 4 Described in siliconising soaking time be 1~2h.
5. the manufacture method of the C/SiC novel mechanical sealing rings according to one of claim 1-4, it is characterised in that step 5 Described in thickness it is smaller 0.08~0.1mm than drawing requirement size.
6. the manufacture method of the C/SiC novel mechanical sealing rings according to one of claim 1-5, it is characterised in that step 6 Described in sedimentation time be 200~300h.
CN201610910155.8A 2016-10-12 2016-10-12 A kind of manufacture method of C/SiC novel mechanical sealing rings Pending CN107445640A (en)

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Cited By (8)

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CN108516852A (en) * 2018-04-08 2018-09-11 中南大学 A kind of carbon-silicon carbide double base matrix carbon fibre composite, preparation method and application
CN108794040A (en) * 2018-06-29 2018-11-13 航天材料及工艺研究所 It is a kind of based on the melting composite material of siliconizing treatment processes, carbon/carbon porous body and preparation method thereof
CN110372408A (en) * 2019-07-23 2019-10-25 中南大学 A kind of ceramic fibre toughening CVD silicon carbide composite material and preparation method and application
CN111333428A (en) * 2020-03-31 2020-06-26 西安鑫垚陶瓷复合材料有限公司 Ceramic matrix composite elastic sealing element and forming process thereof
CN111425598A (en) * 2020-03-31 2020-07-17 西安鑫垚陶瓷复合材料有限公司 Ceramic matrix composite elastic sealing element and forming process thereof
CN111425264A (en) * 2020-03-31 2020-07-17 西安鑫垚陶瓷复合材料有限公司 Ceramic matrix composite elastic sealing element and forming process thereof
CN111517796A (en) * 2020-04-18 2020-08-11 西北工业大学 Ceramic matrix composite elastic sealing element for aero-engine and preparation method thereof
CN114920571A (en) * 2022-05-18 2022-08-19 中国船舶重工集团公司第七二五研究所 Carbon fiber toughened silicon carbide sealing material and preparation method thereof

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CN103724029A (en) * 2013-07-23 2014-04-16 太仓派欧技术咨询服务有限公司 Metal ceramic composite material used at temperature less than 1,200 DEG C
CN103724038A (en) * 2013-09-11 2014-04-16 太仓派欧技术咨询服务有限公司 Preparation method of ceramic matrix hybrid composite material
CN103864451A (en) * 2014-03-26 2014-06-18 西北工业大学 Preparation method of carbon fiber-reinforced ultra high-temperature ceramic-base composite material capable of being repeatedly ablated for use
CN105481429A (en) * 2016-01-11 2016-04-13 山东理工大学 Preparation method of silicon nitride-silicon carbide-carbon fiber friction material

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CN108516852A (en) * 2018-04-08 2018-09-11 中南大学 A kind of carbon-silicon carbide double base matrix carbon fibre composite, preparation method and application
CN108516852B (en) * 2018-04-08 2020-06-26 中南大学 Carbon-silicon carbide binary matrix carbon fiber composite material, and preparation method and application thereof
CN108794040A (en) * 2018-06-29 2018-11-13 航天材料及工艺研究所 It is a kind of based on the melting composite material of siliconizing treatment processes, carbon/carbon porous body and preparation method thereof
CN110372408A (en) * 2019-07-23 2019-10-25 中南大学 A kind of ceramic fibre toughening CVD silicon carbide composite material and preparation method and application
CN111333428A (en) * 2020-03-31 2020-06-26 西安鑫垚陶瓷复合材料有限公司 Ceramic matrix composite elastic sealing element and forming process thereof
CN111425598A (en) * 2020-03-31 2020-07-17 西安鑫垚陶瓷复合材料有限公司 Ceramic matrix composite elastic sealing element and forming process thereof
CN111425264A (en) * 2020-03-31 2020-07-17 西安鑫垚陶瓷复合材料有限公司 Ceramic matrix composite elastic sealing element and forming process thereof
CN111517796A (en) * 2020-04-18 2020-08-11 西北工业大学 Ceramic matrix composite elastic sealing element for aero-engine and preparation method thereof
CN114920571A (en) * 2022-05-18 2022-08-19 中国船舶重工集团公司第七二五研究所 Carbon fiber toughened silicon carbide sealing material and preparation method thereof

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