CN106753196A - A kind of preparation method of high temperature resistant dimensional stability Metal adhesive - Google Patents
A kind of preparation method of high temperature resistant dimensional stability Metal adhesive Download PDFInfo
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- CN106753196A CN106753196A CN201611211681.1A CN201611211681A CN106753196A CN 106753196 A CN106753196 A CN 106753196A CN 201611211681 A CN201611211681 A CN 201611211681A CN 106753196 A CN106753196 A CN 106753196A
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- 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
-
- 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
- C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C09J2483/00—Presence of polysiloxane
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation method of high temperature resistant dimensional stability Metal adhesive, belong to Metal adhesive preparing technical field.The present invention first dries diatom, with nanometer iron powder as catalyst after charing, contained silica reacts at high temperature with charcoal in catalysis diatom, generation silicon carbide whisker, calcined under air conditionses again and remove remaining charcoal, remaining silica is removed using hydrofluoric acid, silicon carbide whisker is purified, as in the phenolic resin that reinforcing agent is modified added to organic siliconresin, high temperature resistant dimensional stability metal adhesive is obtained final product.The present invention is using generation oxidation self-polymeric reaction in the presence of dopamine in aqueous dissolved oxygen, and adhere to silicon carbide whisker surface, improve the compatibility of silicon carbide whisker and phenolic resin, and then the dimensional stability after improving the resistance to elevated temperatures of product and solidifying, efficiently solve the problems, such as conventional metals adhesive resistance to elevated temperatures difference and poor dimensional stability.
Description
Technical field
The invention discloses a kind of preparation method of high temperature resistant dimensional stability Metal adhesive, belong to Metal adhesive
Technical field.
Background technology
It is every with good bond performance, the material that two identical or different solid materials can be linked together is all
It is properly termed as adhesive.It refers to be acted on cohesion etc. by sticking for interface, can make two or more product or material
Natural or synthesis, the organic or inorganic class material that material links together, is also called binder, is traditionally referred to as
Glue.Adhesive with the technology of cohering produces with the generation of human civilization, with the development of human civilization.It is existing
In it is not only widely used in the light and textile industries such as glued board, paper product processing, fiber process, and further promote building, machinery,
The industrial expansions such as aviation, vehicle and shipbuilding；Simultaneously in points such as biomedicine, electronic instrument, defence and military and space technologies
End engineering department also occupies an important position.
Metal is the most widely used structural material of a class, and its connected mode mainly has riveting, welding, threaded connection etc..
Because synthetic adhesive has metal material excellent cohesive action, therefore begin to use adhesive for metal in World War II,
But because past people always suspect and worry, add the combination property for not developing high intensity, high temperature resistant, good endurance
Excellent adhesive, ratio of the adhesive for metal in industrial circle is simultaneously little.
Nowadays, adhesive for metal has gradually obtained the extensive approval of people.Because adhesive for metal is to metal parts
Defect mending and damage maintenance have unique effect, be that common metal processing method is incomparable, cohere in addition not
Malformation and crystalline phase change in organization can be caused because of high-temperature heating as welding, also will not be as riveting, being threadedly coupled because drilling covers
Button causes stress concentration and intensity decreases, thus is used widely.But the weatherability of many Metal adhesives is not on the market
By force, influenced by ambient temperature big, caking property is not strong, and solidification size is unstable, and drying time is long, causes the waste of adhesive.
The content of the invention
The technical problems to be solved by the invention：It is influenced by ambient temperature in use for conventional metals adhesive
Greatly, resistance to elevated temperatures is poor, and caking property is not strong, poor dimensional stability after solidification, the problem for causing metal bond effect poor,
To make modified silicon carbide whisker by oneself it is reinforcing agent there is provided one kind, the phenolic resin compounding being modified with organic siliconresin is obtained resistance to height
The method of warm dimensional stability Metal adhesive.The present invention first dries diatom, with nanometer iron powder as catalyst after charing,
Contained silica is reacted at high temperature with charcoal in catalysis diatom, generates silicon carbide whisker, then removing is calcined under air conditionses
Remaining charcoal, remaining silica is removed using hydrofluoric acid, silicon carbide whisker is purified, and organosilicon is added to as reinforcing agent
In resin modified phenolic resin, high temperature resistant dimensional stability metal adhesive is obtained final product.The present invention is using dopamine in the aqueous solution
There is oxidation self-polymeric reaction in the presence of middle dissolved oxygen, and adhere to silicon carbide whisker surface, improve silicon carbide whisker and phenolic aldehyde
The compatibility of resin, so improve product resistance to elevated temperatures and solidification after dimensional stability, efficiently solve conventional metals
The problem of adhesive resistance to elevated temperatures difference and poor dimensional stability.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）400~600g diatoms are weighed, is placed in baking oven, dried to constant weight under the conditions of being 105~110 DEG C in temperature, then will be dry
Diatom after dry is 100 with nanometer iron powder in mass ratio：1~120：After 1 is well mixed, pour into crucible, then crucible is transferred to
Retort, with 10~20mL/min speed to argon gas is passed through in stove, under argon gas guard mode, with 8~10 DEG C/min speed journeys
Sequence is warming up to 550~600 DEG C, after 20~30min of insulation charing, continue to be warming up to 1400 with 10~15 DEG C/min rate programs~
1500 DEG C, 2~4h of insulation reaction；
（2）Question response terminates, and cools to 700~720 DEG C with the furnace, and then under constant temperature, stopping is passed through argon gas, and with 6~
8mL/min speed terminates to air, 2~3h of insulation reaction, question response is passed through in above-mentioned retort, cools to room temperature with the furnace, and
Material in above-mentioned crucible is poured into filling the plastic tank that 600~800mL mass fractions are 15~20% hydrofluoric acid solutions, immersion
After 30~40min, filtering collects filter cake, and filter cake is washed with deionized until cleaning solution is in neutrality, then filter cake is transferred into baking
In case, dried to constant weight under the conditions of being 105~110 DEG C in temperature, obtain dry cake；
（3）Count by weight, 30~40 parts of above-mentioned gained dry cakes, 10~15 parts of DOPA are sequentially added in there-necked flask
Amine, 150~200 parts of deionized waters, after stirring 3~5min of mixing with glass bar, with 3~5mL/min speed in there-necked flask
Be passed through air, be continually fed into 20~30min, filter, collect filter cake, and filter cake is placed in vacuum drying chamber, in temperature be 60
~65 DEG C of 4~6h of drying, obtain modified silicon carbide whisker, standby；
（4）Count by weight, sequentially add 30~40 part of 1053 organic siliconresin in the there-necked flask of belt stirrer, 10~
15 parts of NaOH, 200~300 parts of deionized waters, then there-necked flask is placed in oil bath pan, in temperature be 110~120 DEG C,
Rotating speed be 300~500r/min under the conditions of, constant temperature 2~4h of stirring reaction, material naturally cools to 80~85 in treating there-necked flask
DEG C, the phenol of 1.6~1.8 times of NaOH quality and the formaldehyde of 1.2~1.4 times of NaOH quality are sequentially added, then
In temperature be 80~85 DEG C, rotating speed be 600~800r/min under the conditions of, 2~4h of constant temperature stirring reaction；
（5）Question response terminates, by material in there-necked flask and step（3）Standby modified silicon carbide whisker is 60 in mass ratio：1~
80：1 adds Rotary Evaporators, is 400~600mmHg in pressure, and temperature is 75~80 DEG C, and rotating speed is 140~160r/min bars
Under part, the 1/6~1/8 of original volume is concentrated under reduced pressure into, discharging is filling after naturally cool to room temperature, obtains final product high temperature resistant dimensionally stable
Type Metal adhesive.
Application process of the invention is：The dust of metal bonding plane, iron rust etc. are removed with clean sand paper first, then with
Acetone cleaning agent is wiped, and metal adhesion surface is cleaned, then by the high temperature resistant dimensional stability Metal adhesive obtained by the present invention
Uniform application is in metal bonding plane and is bonded at once, is then pressed, and is consolidated in the environment of 200~250 DEG C
Change.After testing, the high temperature resistant dimensional stability Metal adhesive stable performance obtained by the present invention, and can tire out at 200~300 DEG C
Meter uses 25000~45000h, can add up to use 300~1500h at 300~500 DEG C, can add up to make at 500~800 DEG C
With 30~45min.
Compared with other method, Advantageous Effects are the present invention：
（1）High temperature resistant dimensional stability Metal adhesive obtained by the present invention has good heat-resisting quantity, and caking property is good, solidification
Good stability of the dimension afterwards is good with metal bond effect；
（2）High temperature resistant dimensional stability Metal adhesive obtained by the present invention has good ermal physics, chemical property, is using work
Under the conditions of work, still possess original performance exposed to high temperature applicationss for a long time, it is heat-resist under temperature cycle change, and can be short
The test of high temperature is born in time.
Specific embodiment
400~600g diatoms are weighed, is placed in baking oven, dried to constant weight under the conditions of being 105~110 DEG C in temperature, then will
Dried diatom is 100 with nanometer iron powder in mass ratio：1~120：After 1 is well mixed, pour into crucible, then crucible is turned
Enter retort, with 10~20mL/min speed to argon gas is passed through in stove, under argon gas guard mode, with 8~10 DEG C/min speed
To 550~600 DEG C, after 20~30min of insulation charing, continuation is warming up to 1400 with 10~15 DEG C/min rate programs for temperature programming
~1500 DEG C, 2~4h of insulation reaction；Question response terminates, and cools to 700~720 DEG C with the furnace, then under constant temperature, stops
Argon gas is passed through, and is terminated to air, 2~3h of insulation reaction, question response is passed through in above-mentioned retort with 6~8mL/min speed, with
Stove is cooled to room temperature, and material in above-mentioned crucible is poured into fills 600~800mL mass fractions for 15~20% hydrofluoric acid solutions
Plastic tank in, after 30~40min of immersion, filter cake is collected in filtering, and filter cake is washed with deionized until cleaning solution is in
Property, then filter cake is transferred in baking oven, dried to constant weight under the conditions of being 105~110 DEG C in temperature, obtain dry cake；By weight
Number meter, sequentially adds 30~40 parts of above-mentioned gained dry cakes in there-necked flask, 10~15 parts of dopamines, and 150~200 parts are gone
Ionized water, after stirring 3~5min of mixing with glass bar, with 3~5mL/min speed to air is passed through in there-necked flask, persistently leads to
Enter 20~30min, filter, collect filter cake, and filter cake is placed in vacuum drying chamber, in temperature be 60~65 DEG C of 4~6h of drying,
Must be modified silicon carbide whisker, standby；Count by weight, 30~40 part 1053 is sequentially added in the there-necked flask of belt stirrer
Organic siliconresin, 10~15 parts of NaOH, 200~300 parts of deionized waters, then there-necked flask is placed in oil bath pan, Yu Wen
It is 110~120 DEG C to spend, under the conditions of rotating speed is 300~500r/min, constant temperature 2~4h of stirring reaction, treat in there-necked flask material from
80~85 DEG C so are cooled to, the phenol and NaOH quality 1.2~1.4 of 1.6~1.8 times of NaOH quality is sequentially added
Times formaldehyde, with after temperature be 80~85 DEG C, rotating speed be 600~800r/min under the conditions of, 2~4h of constant temperature stirring reaction；Treat
Reaction terminates, and is in mass ratio 60 by material in there-necked flask and standby modified silicon carbide whisker：1~80：1 adds rotary evaporation
Instrument, in pressure be 400~600mmHg, temperature be 75~80 DEG C, rotating speed be 140~160r/min under the conditions of, be concentrated under reduced pressure into original
The 1/6~1/8 of volume, discharging is filling after naturally cool to room temperature, obtains final product high temperature resistant dimensional stability Metal adhesive.
Example 1
Weigh 400g diatoms, be placed in baking oven, in temperature be 105 DEG C under the conditions of dry to constant weight, then by dried diatom with
Nanometer iron powder is 100 in mass ratio：1：After 1 is well mixed, pour into crucible, then crucible is transferred to retort, with 10mL/min
Speed under argon gas guard mode, 550 DEG C, insulation charing is warming up to 8 DEG C/min rate programs to argon gas is passed through in stove
After 20min, continuation is warming up to 1400 DEG C, insulation reaction 2h with 10 DEG C/min rate programs；Question response terminates, and cools to the furnace
700 DEG C, then under constant temperature, stopping is passed through argon gas, and is protected to air is passed through in above-mentioned retort with 6mL/min speed
Temperature reaction 2h, question response terminates, and cools to room temperature with the furnace, and material in above-mentioned crucible is poured into fills 600mL mass fractions and be
In the plastic tank of 15% hydrofluoric acid solution, after immersion 30min, filtering collects filter cake, and filter cake is washed with deionized until washing
Liquid is washed in neutrality, then filter cake is transferred in baking oven, dried to constant weight under the conditions of being 105 DEG C in temperature, obtain dry cake；By weight
Number meter, sequentially adds 30 parts of above-mentioned gained dry cakes in there-necked flask, and 10 parts of dopamines, 150 parts of deionized waters use glass
After glass rod stirring mixing 3min, with 3mL/min speed to air is passed through in there-necked flask, 20min is continually fed into, filtered, collected
Filter cake, and filter cake is placed in vacuum drying chamber, 4h is dried for 60 DEG C in temperature, obtains modified silicon carbide whisker, standby；By weight
Number meter, sequentially adds 30 part of 1053 organic siliconresin in the there-necked flask of belt stirrer, 10 parts of NaOH, and 200 parts are gone
Ionized water, then there-necked flask is placed in oil bath pan, it is 110 DEG C in temperature, rotating speed is under the conditions of 300r/min, constant temperature stirring is anti-
2h is answered, material naturally cools to 80 DEG C in treating there-necked flask, sequentially add the phenol and hydroxide of 1.6 times of NaOH quality
The formaldehyde that 1.2 times of sodium quality, with after temperature be 80 DEG C, rotating speed be 600r/min under the conditions of, constant temperature stirring reaction 2h；Question response
Terminate, be in mass ratio 60 by material in there-necked flask and standby modified silicon carbide whisker：1：1 adds Rotary Evaporators, in pressure
Power is 400mmHg, and temperature is 75 DEG C, and under the conditions of 140r/min, to be concentrated under reduced pressure into the 1/6 of original volume, nature is treated in discharging to rotating speed
Room temperature is cooled to, it is filling, obtain final product high temperature resistant dimensional stability Metal adhesive.
The dust of metal bonding plane, iron rust etc. are removed with clean sand paper first, then is wiped with acetone cleaning agent, cleaning
Metal adhesion surface, then by the high temperature resistant dimensional stability Metal adhesive uniform application obtained by the present invention in metal bonding plane
And bonded at once, then pressed, and solidified in the environment of 200 DEG C.After testing, the resistance to height obtained by the present invention
Warm dimensional stability Metal adhesive stable performance, and can add up to use 25000h at 200 DEG C, can add up to make at 300 DEG C
With 300h, can add up to use 30min at 500 DEG C.
Example 2
Weigh 600g diatoms, be placed in baking oven, in temperature be 110 DEG C under the conditions of dry to constant weight, then by dried diatom with
Nanometer iron powder is 100 in mass ratio：120：After 1 is well mixed, pour into crucible, then crucible is transferred to retort, with 20mL/
Min speed under argon gas guard mode, 600 DEG C, insulation charing is warming up to 10 DEG C/min rate programs to argon gas is passed through in stove
After 30min, continuation is warming up to 1500 DEG C, insulation reaction 4h with 15 DEG C/min rate programs；Question response terminates, and cools to the furnace
720 DEG C, then under constant temperature, stopping is passed through argon gas, and is protected to air is passed through in above-mentioned retort with 8mL/min speed
Temperature reaction 3h, question response terminates, and cools to room temperature with the furnace, and material in above-mentioned crucible is poured into fills 800mL mass fractions and be
In the plastic tank of 20% hydrofluoric acid solution, after immersion 40min, filtering collects filter cake, and filter cake is washed with deionized until washing
Liquid is washed in neutrality, then filter cake is transferred in baking oven, dried to constant weight under the conditions of being 110 DEG C in temperature, obtain dry cake；By weight
Number meter, sequentially adds 40 parts of above-mentioned gained dry cakes in there-necked flask, and 15 parts of dopamines, 200 parts of deionized waters use glass
After glass rod stirring mixing 5min, with 5mL/min speed to air is passed through in there-necked flask, 30min is continually fed into, filtered, collected
Filter cake, and filter cake is placed in vacuum drying chamber, 6h is dried for 65 DEG C in temperature, obtains modified silicon carbide whisker, standby；By weight
Number meter, sequentially adds 40 part of 1053 organic siliconresin in the there-necked flask of belt stirrer, 15 parts of NaOH, and 300 parts are gone
Ionized water, then there-necked flask is placed in oil bath pan, it is 120 DEG C in temperature, rotating speed is under the conditions of 500r/min, constant temperature stirring is anti-
4h is answered, material naturally cools to 85 DEG C in treating there-necked flask, sequentially add the phenol and hydroxide of 1.8 times of NaOH quality
The formaldehyde that 1.4 times of sodium quality, with after temperature be 85 DEG C, rotating speed be 800r/min under the conditions of, constant temperature stirring reaction 4h；Question response
Terminate, be in mass ratio 60 by material in there-necked flask and standby modified silicon carbide whisker：80：1 adds Rotary Evaporators, in pressure
Power is 600mmHg, and temperature is 80 DEG C, and under the conditions of 160r/min, to be concentrated under reduced pressure into the 1/8 of original volume, nature is treated in discharging to rotating speed
Room temperature is cooled to, it is filling, obtain final product high temperature resistant dimensional stability Metal adhesive.
The dust of metal bonding plane, iron rust etc. are removed with clean sand paper first, then is wiped with acetone cleaning agent, cleaning
Metal adhesion surface, then by the high temperature resistant dimensional stability Metal adhesive uniform application obtained by the present invention in metal bonding plane
And bonded at once, then pressed, and solidified in the environment of 250 DEG C.After testing, the resistance to height obtained by the present invention
Warm dimensional stability Metal adhesive stable performance, and can add up to use 45000h at 300 DEG C, can add up to make at 500 DEG C
With 1500h, can add up to use 45min at 800 DEG C.
Example 3
Weigh 500g diatoms, be placed in baking oven, in temperature be 107 DEG C under the conditions of dry to constant weight, then by dried diatom with
Nanometer iron powder is 100 in mass ratio：60：After 1 is well mixed, pour into crucible, then crucible is transferred to retort, with 15mL/min
Speed under argon gas guard mode, 575 DEG C, insulation charing is warming up to 9 DEG C/min rate programs to argon gas is passed through in stove
After 25min, continuation is warming up to 1450 DEG C, insulation reaction 3h with 13 DEG C/min rate programs；Question response terminates, and cools to the furnace
710 DEG C, then under constant temperature, stopping is passed through argon gas, and is protected to air is passed through in above-mentioned retort with 7mL/min speed
Temperature reaction 3h, question response terminates, and cools to room temperature with the furnace, and material in above-mentioned crucible is poured into fills 700mL mass fractions and be
In the plastic tank of 17% hydrofluoric acid solution, after immersion 35min, filtering collects filter cake, and filter cake is washed with deionized until washing
Liquid is washed in neutrality, then filter cake is transferred in baking oven, dried to constant weight under the conditions of being 108 DEG C in temperature, obtain dry cake；By weight
Number meter, sequentially adds 35 parts of above-mentioned gained dry cakes in there-necked flask, and 13 parts of dopamines, 175 parts of deionized waters use glass
After glass rod stirring mixing 4min, with 4mL/min speed to air is passed through in there-necked flask, 25min is continually fed into, filtered, collected
Filter cake, and filter cake is placed in vacuum drying chamber, 5h is dried for 63 DEG C in temperature, obtains modified silicon carbide whisker, standby；By weight
Number meter, sequentially adds 35 part of 1053 organic siliconresin in the there-necked flask of belt stirrer, 13 parts of NaOH, and 250 parts are gone
Ionized water, then there-necked flask is placed in oil bath pan, it is 115 DEG C in temperature, rotating speed is under the conditions of 400r/min, constant temperature stirring is anti-
3h is answered, material naturally cools to 83 DEG C in treating there-necked flask, sequentially add the phenol and hydroxide of 1.7 times of NaOH quality
The formaldehyde that 1.3 times of sodium quality, with after temperature be 82 DEG C, rotating speed be 700r/min under the conditions of, constant temperature stirring reaction 3h；Question response
Terminate, be in mass ratio 60 by material in there-necked flask and standby modified silicon carbide whisker：40：1 adds Rotary Evaporators, in pressure
Power is 500mmHg, and temperature is 77 DEG C, and under the conditions of 150r/min, to be concentrated under reduced pressure into the 1/7 of original volume, nature is treated in discharging to rotating speed
Room temperature is cooled to, it is filling, obtain final product high temperature resistant dimensional stability Metal adhesive.
The dust of metal bonding plane, iron rust etc. are removed with clean sand paper first, then is wiped with acetone cleaning agent, cleaning
Metal adhesion surface, then by the high temperature resistant dimensional stability Metal adhesive uniform application obtained by the present invention in metal bonding plane
And bonded at once, then pressed, and solidified in the environment of 225 DEG C.After testing, the resistance to height obtained by the present invention
Warm dimensional stability Metal adhesive stable performance, and can add up to use 35000h at 250 DEG C, can add up to make at 400 DEG C
With 900h, can add up to use 40min at 650 DEG C.
Claims (1)
1. a kind of preparation method of high temperature resistant dimensional stability Metal adhesive, it is characterised in that specific preparation process is：
（1）400~600g diatoms are weighed, is placed in baking oven, dried to constant weight under the conditions of being 105~110 DEG C in temperature, then will be dry
Diatom after dry is 100 with nanometer iron powder in mass ratio：1~120：After 1 is well mixed, pour into crucible, then crucible is transferred to
Retort, with 10~20mL/min speed to argon gas is passed through in stove, under argon gas guard mode, with 8~10 DEG C/min speed journeys
Sequence is warming up to 550~600 DEG C, after 20~30min of insulation charing, continue to be warming up to 1400 with 10~15 DEG C/min rate programs~
1500 DEG C, 2~4h of insulation reaction；
（2）Question response terminates, and cools to 700~720 DEG C with the furnace, and then under constant temperature, stopping is passed through argon gas, and with 6~
8mL/min speed terminates to air, 2~3h of insulation reaction, question response is passed through in above-mentioned retort, cools to room temperature with the furnace, and
Material in above-mentioned crucible is poured into filling the plastic tank that 600~800mL mass fractions are 15~20% hydrofluoric acid solutions, immersion
After 30~40min, filtering collects filter cake, and filter cake is washed with deionized until cleaning solution is in neutrality, then filter cake is transferred into baking
In case, dried to constant weight under the conditions of being 105~110 DEG C in temperature, obtain dry cake；
（3）Count by weight, 30~40 parts of above-mentioned gained dry cakes, 10~15 parts of DOPA are sequentially added in there-necked flask
Amine, 150~200 parts of deionized waters, after stirring 3~5min of mixing with glass bar, with 3~5mL/min speed in there-necked flask
Be passed through air, be continually fed into 20~30min, filter, collect filter cake, and filter cake is placed in vacuum drying chamber, in temperature be 60
~65 DEG C of 4~6h of drying, obtain modified silicon carbide whisker, standby；
（4）Count by weight, sequentially add 30~40 part of 1053 organic siliconresin in the there-necked flask of belt stirrer, 10~
15 parts of NaOH, 200~300 parts of deionized waters, then there-necked flask is placed in oil bath pan, in temperature be 110~120 DEG C,
Rotating speed be 300~500r/min under the conditions of, constant temperature 2~4h of stirring reaction, material naturally cools to 80~85 in treating there-necked flask
DEG C, the phenol of 1.6~1.8 times of NaOH quality and the formaldehyde of 1.2~1.4 times of NaOH quality are sequentially added, then
In temperature be 80~85 DEG C, rotating speed be 600~800r/min under the conditions of, 2~4h of constant temperature stirring reaction；
（5）Question response terminates, by material in there-necked flask and step（3）Standby modified silicon carbide whisker is 60 in mass ratio：1~
80：1 adds Rotary Evaporators, is 400~600mmHg in pressure, and temperature is 75~80 DEG C, and rotating speed is 140~160r/min bars
Under part, the 1/6~1/8 of original volume is concentrated under reduced pressure into, discharging is filling after naturally cool to room temperature, obtains final product high temperature resistant dimensionally stable
Type Metal adhesive.
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| CN109231949A (en) * | 2018-11-19 | 2019-01-18 | 中国民航大学 | Silicon carbide whisker is directly mixed and growth in situ coordination plasticizing type high-temperature plastic preparation method |
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| CN107540874A (en) * | 2017-07-31 | 2018-01-05 | 常州市卜诺赛机电技术有限公司 | A kind of preparation method of the dedicated modified talcum powder of polypropylene plastics |
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| CN109231949A (en) * | 2018-11-19 | 2019-01-18 | 中国民航大学 | Silicon carbide whisker is directly mixed and growth in situ coordination plasticizing type high-temperature plastic preparation method |
| CN110483053A (en) * | 2019-09-25 | 2019-11-22 | 哈尔滨工业大学 | A kind of SiC nanowire/SiC porous ceramics preparation method for inhaling wave for high temperature |
| CN110483053B (en) * | 2019-09-25 | 2021-08-20 | 哈尔滨工业大学 | Preparation method of SiC nanowire/SiC porous ceramic for high-temperature wave absorption |
| CN113620298A (en) * | 2021-08-13 | 2021-11-09 | 中国科学院广州地球化学研究所 | Diatom-based silicon carbide material and preparation method and application thereof |
| CN113620298B (en) * | 2021-08-13 | 2022-12-02 | 中国科学院广州地球化学研究所 | Diatom-based silicon carbide material and preparation method and application thereof |
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