CN105419726B - A kind of copna resin binding agent and preparation method, application method - Google Patents
A kind of copna resin binding agent and preparation method, application method Download PDFInfo
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- CN105419726B CN105419726B CN201510975776.XA CN201510975776A CN105419726B CN 105419726 B CN105419726 B CN 105419726B CN 201510975776 A CN201510975776 A CN 201510975776A CN 105419726 B CN105419726 B CN 105419726B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J195/00—Adhesives based on bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The present invention relates to a kind of copna resin binding agent and preparation method, application method, the binding agent includes copna resin and modified filler, and the copna resin includes：45~55wt.% pitch powder, 35~45wt.% terephthalyl alcohol, 5~10wt.% p-methyl benzenesulfonic acid；The modified filler includes：To account for the copna resin total amount percentages, 5~10wt.% boron carbide powder and 1~2wt.% short carbon fibers；The binding agent preparation method includes：Prepare copna resin and copna resin is modified；The application method of the binding agent includes：Object is bonded, is heat-treated and CVD deposition.The binding agent not only has high bond strength, heat resistance and thermal shock resistance, while having the performance for keeping physicochemical property to be basically unchanged in high temperature environments.
Description
Technical field
The present invention relates to high-temperature agglomerant technical field, more particularly to a kind of copna resin binding agent and preparation method, make
Use method.
Background technology
Copna resin is to be invented by Japanese large space between muscles China fir youth et al. in last century the eighties and is Novel hot of concern
Solidity organic resin.The characteristics of it is maximum is not present containing long-chain fat race structures more than two carbon in structure, therefore is had
Excellent resistance to elevated temperatures, while the intermediate product B rank copna resin good fluidities that preparation process is produced, facilitate technological operation,
Therefore it is widely used in high temperature bond field.Wherein asphaltic base copna resin has especially high carbon yield and β resin contents,
Adhesion strength is high, and be used for superhigh temperature composite bonds industry, but is cracked in copna resin heat treatment process,
Constantly discharge CO, H2O、O2Etc. oxygen-containing small molecule, and with the rise of temperature, the amount and speed of release are all constantly raised, led
Cause to occur in volume contraction, glue-line to need when micropore and crackle, mechanical properties decrease, therefore copna resin are used as binding agent
It is modified.
The content of the invention
In view of above-mentioned analysis, the present invention is intended to provide a kind of copna resin binding agent and preparation method, application method,
The binding agent not only has high bond strength, heat resistance and thermal shock resistance, while having higher holding physics and chemistry in high temperature environments
The performance that performance is basically unchanged.
The purpose of the present invention is mainly achieved through the following technical solutions：
A kind of copna resin binding agent of the present invention, including copna resin and modified filler, the copna resin include：
45~55wt.% pitch powder, 35~45wt.% terephthalyl alcohol, 5~10wt.% p-methyl benzenesulfonic acid；The modification
Filler includes：To account for the copna resin total amount percentages, the 5~10wt.% chopped charcoal of boron carbide powder and 1~2wt.%
Fiber.
A kind of preparation method of copna resin binding agent of the present invention, it is characterised in that comprise the following steps：
First, copna resin is prepared：A certain amount of pitch powder, terephthalyl alcohol are weighed according to copna resin matching principle
And p-methyl benzenesulfonic acid, it will be put into after the pitch powder ball milling in three-necked flask, while adding the terephthalyl alcohol and described
P-methyl benzenesulfonic acid, is slowly heated to 250 DEG C~300 DEG C, it is ensured that reaction can be carried out gently, insulation material into the three-necked flask
In complete molten condition, complete copna resin and prepare；
Then, copna resin is modified：The amount of copna resin is weighed and prepared according to modified filler matching principle
Corresponding boron carbide powder and short carbon fiber, the three-necked flask is added by the boron carbide powder and the short carbon fiber
In, it is incubated to the modified filler and is uniformly mixed with the copna resin at 250 DEG C~300 DEG C, completes copna resin and glue
Agent is tied to prepare.
Further, in the step of preparing copna resin, the pitch powder ball milling arrived 200 mesh sieves.
Further, in the step of preparing copna resin, insulation material into the three-necked flask is in complete molten condition
During, it is necessary to be stirred continuously, while instill acetone, the acetone infusion volume is the shape that just keeps solution to be provoked by glass bar
State.
Further, in the step of being modified to copna resin, insulation to the modified filler and the COPNA trees
, it is necessary to be stirred continuously in the uniform mixed process of fat, while instilling acetone, the acetone infusion volume is just holding solution by glass
The state that rod is provoked.
Copna resin Binder Composition of the present invention is illustrated：
(1) copna resin each component explanation：
Asphaltic base copna resin has especially high carbon yield and β resin contents, with high strength bond power, therefore this
Invention is from monomer of the pitch powder as copna resin；
Terephthalyl alcohol is the crosslinking agent of copna resin, and bridging action is played between coal tar pitch monomer, promotes coal tar pitch monomer
It is cross-linked with each other and condenses together；
P-methyl benzenesulfonic acid is the catalyst of copna resin, promotes each material in copna resin to react to each other.
(2) modified filler each component explanation：
Copna resin is heated to be cracked, and constantly discharges CO, H2O、O2Etc. oxygen-containing small molecule, and with the liter of temperature
Height, the amount and speed of release are all constantly raised, and are caused micropore and crackle occur in volume contraction, copna resin, are ultimately resulted in power
Learn hydraulic performance decline.
B is added in copna resin4C (boron carbide) particle, there is good modified effect：
At 500~600 DEG C, B4C and the oxygen-containing small molecule of release are reacted by procedure below and generate B2O3：
B4C+6CO=2B2O3+7C
B4C+(8-x)H2O=2B2O3+xCO+(1-x)CO2+(8-x)H2
X is the CO and CO that are generated2The CO of mixed gas volume fraction, span is 0~1.
B4C is to B2O3Conversion, volumetric expansion about 250% can be alleviated in COPNA thermal histories caused by volume contraction
Thermal stress；The B generated simultaneously2O3Fusing point be only 450 DEG C, it is good with the wellability of resin matrix, when matrix produces micro-crack,
B2O3It is movable at micro-crack and makes crackle up.
Short carbon fiber is added in copna resin, there is good modified effect：
Carbon fibe intensity is high, and thermal shock resistance is good, good with resin charing product compatibility, therefore adds in a binder suitable
Short carbon fiber is measured, adhesive strength and toughness can be effectively improved.When binder substrate is broken, short carbon fiber bears outer
Boundary's load is simultaneously built bridge between the crack surface of disconnection, plays " bridge joint " effect；When short carbon fiber under extraneous load effect from
Extracted in matrix, toughened and reinforced purpose is reached because of the energy that interface friction consumes extraneous load.
A kind of application method of copna resin binding agent of the present invention, including object are bonded, are heat-treated and CVD deposition step,
It is specific as follows：
(1) object is bonded：Object face to be bonded is pre-processed into the reeded face of tool, then the copna resin is glued
Knot agent is coated on the face to be bonded, and two face docking to be bonded are bonded, while being fixed with fixture；
(2) it is heat-treated：The object after bonding is put into heating furnace, with 5~10 DEG C/min speed under protective atmosphere
Rate is heated to 350 DEG C and is incubated after 2h, and continuation is heated to 1700 DEG C with 5~10 DEG C/min speed and is incubated 2h, then in stove
The interior speed with 5~10 DEG C/min is cooled to room temperature；
(3) CVD deposition：The object after heat treatment is put into chemical vapor deposition stove, methane and propane mixing is passed through
Gas, is incubated 10h~15h at 1500~2000 DEG C, cools to the furnace after room temperature and takes out, completes deposition process, CVD deposition energy
The hole that enough filling copna resin binding agent is produced because charing causes volume contraction, improves the cohesive strength of binding agent.
Further, face preprocess method to be bonded is in the step (1)：Polished the face to be bonded with sand paper, so
The uniform fluting on the face to be bonded afterwards, the groove is in latticed on face to be bonded, and the depth of groove is 0.5mm,
Then the face to be bonded is placed in sonic oscillation in alcohol, dry, wherein the groove can increase binding agent with it is to be bonded
The contact area in face, while producing physics " pin-spoon " effect, occurs plasticity and becomes during the binding agent stress being forced into groove
Shape, absorbs energy, so as to increase adhesive strength and plasticity.
Further, protective atmosphere is nitrogen in the step (2), and the nitrogen flow is 50~100ml/min.
Further, methane and propane ratio are 2 in methane and propane mixture body in the step (3):1~4:1.
The present invention has the beneficial effect that：
The present invention adds boron carbide powder and short carbon fiber modified filler, boron carbide powder in asphaltic base copna resin
Grain slows down resin and produces volume contraction because heated, makes up micro-crack, while short carbon fiber can then pass through bridge joint and spike protein gene
Mechanism produces toughening effect to resinoid bond, CVD is coordinated when using, further repairing binder is produced because of volume contraction
Cavity, while the advantage of asphaltic base copna resin is ensured, the further bonding for improving binding agent is strong, high temperature resistant, anti-thermal shock
The performance that higher holding physicochemical property is basically unchanged under property and high temperature.The binding agent shear strength that the present invention is provided is up to
15Mpa, the 2h mechanical properties that worked at 1500 DEG C are held essentially constant, and still keep certain after 1500 DEG C of thermal cycles 100 times
Shear strength, tack coat occurs without obvious crackle.
Other features and advantages of the present invention will be illustrated in the following description, also, the partial change from specification
Obtain it is clear that or being understood by implementing the present invention.The purpose of the present invention and other advantages can be by the explanations write
Specifically noted structure is realized and obtained in book, claims and accompanying drawing.
Brief description of the drawings
Accompanying drawing is only used for showing the purpose of specific embodiment, and is not considered as limitation of the present invention, in whole accompanying drawing
In, identical reference symbol represents identical part.
Fig. 1 is copna resin binding agent preparation facilities of the present invention,
Wherein 1 heater, 2 agitating devices, 3 three-necked flasks, 4 burets, 5 reflux condensing tubes.
Embodiment
The preferred embodiments of the present invention are specifically described below in conjunction with the accompanying drawings, wherein, accompanying drawing constitutes the application part, and
It is used for the principle for explaining the present invention together with embodiments of the present invention.
Pitch powder of the present invention, nitrogen, methane and propane are industrial standards；
The terephthalyl alcohol, p-methyl benzenesulfonic acid, acetone are the pure standard of analysis；
Described boron carbide powder granularity is 200-300 mesh；
7 μm of described short carbon fiber diameter, length is 50-100 μm.
Embodiment 1
The present invention prepares a kind of copna resin binding agent, including copna resin and modified filler, wherein the COPNA trees
Fat includes：45wt.% pitch powder, 45wt.% terephthalyl alcohol, 10wt.% p-methyl benzenesulfonic acid；The modified filler
Including：To account for the copna resin total amount percentages, 5wt.% boron carbide powder and 1wt.% short carbon fibers.
The preparation method of the binding agent, comprises the following steps：
First, copna resin is prepared：According to copna resin matching principle weigh 45wt.% pitch powders, 45wt.% pairs
Benzene dimethanol and 10wt.% p-methyl benzenesulfonic acid, the pitch powder ball milling is crossed after 200 mesh sieves and is put into three mouthfuls by charging aperture 6
In flask 3, while adding the terephthalyl alcohol and the p-methyl benzenesulfonic acid, then 250 are slowly heated to heater 1
DEG C, the reaction in three-necked flask 3 is gently carried out, then in 250 DEG C of insulations, agitating device 2 is from charging aperture 6 during insulation
Insert in three-necked flask 3, solution is stirred, and acetone is instilled from buret 4, material has been in into the three-necked flask
Full-fusing state, the acetone infusion volume is the state for just keeping solution to be provoked by glass bar, completes copna resin and prepares；
Then, copna resin is modified：Weighed according to modified filler matching principle and account for the copna resin
5wt.% boron carbide powders and 1wt.% short carbon fibers, then take out agitating device 2, by the boron carbide powder and the chopped charcoal
Fiber is added in the three-necked flask 3 from charging aperture 6, is then inserted agitating device 2 in three-necked flask 3 from charging aperture, is kept
The temperature of three-necked flask 3 is 250 DEG C and to be incubated, and is constantly stirred in insulating process with agitating device 2, while by acetone from drop
Fixed tube 4 is instilled, and accelerates material in three-necked flask 3 uniformly to mix, until the modified filler is uniformly mixed with the copna resin
Close, complete copna resin binding agent and prepare.
Material can volatilize because heated in three-necked flask 3 in preparation process, the material of volatilization when by reflux condensing tube 5,
Solution is condensed into again by the cooling effect of cooling water to flow back in the three-necked flask 3, it is ensured that according to copna resin binding agent
It is prepared by matching principle.
The copna resin binding agent of preparation is bonded for object, its application method comprises the following steps：
(1) object is bonded：Object face to be bonded is polished with sand paper, then the uniform fluting on the face to be bonded,
It is in latticed on the bonding plane to make the groove, and depth of groove is 0.5mm, then face to be bonded is placed in alcohol ultrasonic
Vibration, drying, then applies the copna resin binding agent on the face to be bonded, and two face docking to be bonded are bonded, simultaneously
Fixed with graphite fixture；
(2) it is heat-treated：The object after bonding is put into heating furnace, added in a nitrogen atmosphere with 5 DEG C/min speed
Heat is to 350 DEG C and is incubated 2h, wherein the nitrogen flow is 50ml/min, then proceedes to be heated to 5 DEG C/min speed
1700 DEG C and 2h is incubated, room temperature is then cooled to 5 DEG C/min speed in stove；
(3) CVD deposition：The object after heat treatment is put into chemical vapor deposition stove, methane is passed through and propane ratio is
4:1 mixed gas, 15h is incubated at 1500 DEG C, is cooled to the furnace after room temperature and is taken out, CVD deposition can fill copna resin
The hole that binding agent is produced because charing causes volume contraction, improves the cohesive strength of binding agent.
Performance evaluation is carried out to the binding agent of embodiment 1, carried out in such a way：
(1) shear strength：The cutting performance of test sample reaches 15.5Mpa on universal electrical sample machine, meets to use and wants
Ask.
(2) heat resistance：The shear strength of sample test sample on universal electrical sample machine after 1500 DEG C of insulation 2h
For 13.9MPa, meet use requirement.
(3) thermal shock resistance：Sample is put into Si-Mo rod stove at 1500 DEG C and is incubated 10 minutes, natural cooling is then taken out
To room temperature, circulate 100 times.The shear strength of test sample is 12.0Mpa on universal electrical sample machine, meets use requirement.
Embodiment 2
The present invention prepares a kind of copna resin binding agent, including copna resin and modified filler, wherein the COPNA trees
Fat includes：55wt.% pitch powder, 35wt.% terephthalyl alcohol, 10wt.% p-methyl benzenesulfonic acid；The modified filler
Including：To account for the copna resin total amount percentages, 10wt.% boron carbide powder and 2wt.% short carbon fibers.
The preparation method of the binding agent, comprises the following steps：
First, copna resin is prepared：According to copna resin matching principle weigh 55wt.% pitch powders, 35wt.% pairs
Benzene dimethanol and 10wt.% p-methyl benzenesulfonic acid, the pitch powder ball milling is crossed after 200 mesh sieves and is put into three mouthfuls by charging aperture 6
In flask 3, while adding the terephthalyl alcohol and the p-methyl benzenesulfonic acid, then 300 are slowly heated to heater 1
DEG C, the reaction in three-necked flask 3 is gently carried out, then in 300 DEG C of insulations, agitating device 2 is from charging aperture 6 during insulation
Insert in three-necked flask 3, solution is stirred, and acetone is instilled from buret 4, material is in into the three-necked flask 3
Complete molten condition, the acetone infusion volume is the state for just keeping solution to be provoked by glass bar, completes copna resin system
It is standby；
Then, copna resin is modified：Weighed according to modified filler matching principle and account for the copna resin
10wt.% boron carbide powders and 2wt.% short carbon fibers then take out agitating device 2, by the boron carbide powder and the chopped charcoal
Fiber is added in the three-necked flask 3 from charging aperture 6, is then inserted agitating device 2 in three-necked flask 3 from charging aperture, is kept
The temperature of three-necked flask 3 is 300 DEG C and to be incubated, and is constantly stirred in insulating process with agitating device 2, while by acetone from drop
Fixed tube 4 is instilled, and accelerates material in three-necked flask 3 uniformly to mix, until the modified filler is uniformly mixed with the copna resin
Close, complete copna resin binding agent and prepare.
Material can volatilize because heated in three-necked flask 3 in preparation process, the material of volatilization when by reflux condensing tube 5,
Solution is condensed into again by the cooling effect of cooling water to flow back in the three-necked flask 3, it is ensured that according to copna resin binding agent
It is prepared by matching principle.
The copna resin binding agent of preparation is bonded for object, its application method comprises the following steps：
(1) object is bonded：Object face to be bonded is polished with sand paper, then the uniform fluting on the face to be bonded,
It is in latticed on the bonding plane to make the groove, and depth of groove is 0.5mm, then face to be bonded is placed in alcohol ultrasonic
Vibration, drying, then applies the copna resin binding agent on the face to be bonded, and two face docking to be bonded are bonded, simultaneously
Fixed with graphite fixture；
(2) it is heat-treated：The object after bonding is put into heating furnace, added in a nitrogen atmosphere with 10 DEG C/min speed
Heat is to 350 DEG C and is incubated 2h, wherein the nitrogen flow is 50ml/min, then proceedes to be heated to 10 DEG C/min speed
1700 DEG C and 2h is incubated, room temperature is then cooled to 10 DEG C/min speed in stove；
(3) CVD deposition：The object after heat treatment is put into chemical vapor deposition stove, methane is passed through and propane ratio is
2:1 mixed gas, 10h is incubated at 2000 DEG C and cools to taking-up after room temperature with the furnace, CVD deposition can fill copna resin
The hole that binding agent is produced because charing causes volume contraction, improves the cohesive strength of binding agent.
Performance evaluation is carried out to the binding agent of embodiment 2, carried out in such a way：
(1) shear strength：The cutting performance of test sample reaches 14.9Mpa on universal electrical sample machine, meets to use and wants
Ask.
(2) heat resistance：The shear strength of sample test sample on universal electrical sample machine after 1500 DEG C of insulation 2h
For 14MPa, meet use requirement.
(3) thermal shock resistance：Sample is put into Si-Mo rod stove at 1500 DEG C and is incubated 10 minutes, natural cooling is then taken out
To room temperature, circulate 100 times.The shear strength of test sample is 11Mpa on universal electrical sample machine, meets use requirement.
In summary, the embodiments of the invention provide a kind of copna resin binding agent and preparation method, application method,
While ensureing the advantage of asphaltic base copna resin, the bonding that further improves binding agent is strong, high temperature resistant, thermal shock resistance and height
The performance that higher holding physicochemical property is basically unchanged under temperature.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.
Claims (6)
1. a kind of copna resin binding agent, it is characterised in that including copna resin and modified filler, the copna resin is closed
Include into raw material：45~55wt.% pitch powder, 35~45wt.% terephthalyl alcohol, 5~10wt.% to toluene sulphur
Acid；The modified filler includes：To account for the copna resin total amount percentages, 5~10wt.% boron carbide powder and 1~
2wt.% short carbon fibers；A diameter of 7 μm of the short carbon fiber, length is 50-100 μm；
Its preparation comprises the following steps：
First, copna resin is prepared：A certain amount of pitch powder, terephthalyl alcohol and right are weighed according to copna resin matching principle
Toluenesulfonic acid, will be put into three-necked flask after the pitch powder ball milling, while adding the terephthalyl alcohol and described to first
Benzene sulfonic acid, is slowly heated to 250 DEG C~300 DEG C, insulation material into the three-necked flask is in complete molten condition, is completed
It is prepared by copna resin；In the step of preparing copna resin, insulation material into the three-necked flask is in complete molten condition mistake
, it is necessary to be stirred continuously in journey, while instilling acetone, the acetone infusion volume is just to keep the shape that solution is provoked by glass bar
State；
Then, copna resin is modified：Weighed according to modified filler matching principle relative with the amount for preparing copna resin
The boron carbide powder and short carbon fiber answered, the boron carbide powder and the short carbon fiber are added in the three-necked flask,
It is incubated to the modified filler and is uniformly mixed with the copna resin at 250 DEG C~300 DEG C, completes copna resin binding agent system
It is standby；
In the step of being modified to copna resin, insulation to the modified filler and the uniform mixed process of the copna resin
In, it is necessary to be stirred continuously, while instill acetone, the acetone infusion volume is the state that just keeps solution to be provoked by glass bar.
2. copna resin binding agent according to claim 1, it is characterised in that in the step of preparing copna resin, institute
State pitch powder ball milling and arrive 200 mesh sieves.
3. a kind of application method of copna resin binding agent as claimed in claim 1, it is characterised in that including object bonding, heat
Processing and CVD deposition step, it is specific as follows：
(1) object is bonded：Object face to be bonded is pre-processed into the reeded face of tool, then by the copna resin binding agent
It is coated on the face to be bonded, two face docking to be bonded are bonded, while being fixed with fixture；
(2) it is heat-treated：The object after bonding is put into heating furnace, added under protective atmosphere with 5~10 DEG C/min speed
Heat is to 350 DEG C and is incubated after 2h, and continuation is heated to 1700 DEG C with 5~10 DEG C/min speed and is incubated 2h, then with 5 in stove
~10 DEG C/min speed is cooled to room temperature；
(3) CVD deposition：The object after heat treatment is put into chemical vapor deposition stove, methane and propane mixture body is passed through,
10h~15h is incubated at 1500~2000 DEG C, cools to the furnace after room temperature and takes out, complete deposition process.
4. the application method of copna resin binding agent according to claim 3, it is characterised in that wait to glue in the step (1)
Junction preprocess method is：With the sand paper polishing face to be bonded, then the uniform fluting on the face to be bonded, described recessed
Groove is in latticed on face to be bonded, and the depth of groove is 0.5mm, and the face to be bonded then is placed in into ultrasound in alcohol and shaken
Swing, dry.
5. the application method of copna resin binding agent according to claim 3, it is characterised in that protected in the step (2)
Atmosphere is nitrogen, and the nitrogen flow is 50~100ml/min.
6. the application method of copna resin binding agent according to claim 3, it is characterised in that methane in the step (3)
It is 2 with methane in propane mixture body and propane ratio:1~4:1.
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