CN108558268A - A kind of fibre reinforced high temperature resistant adhesive and preparation method thereof - Google Patents
A kind of fibre reinforced high temperature resistant adhesive and preparation method thereof Download PDFInfo
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- CN108558268A CN108558268A CN201810653960.6A CN201810653960A CN108558268A CN 108558268 A CN108558268 A CN 108558268A CN 201810653960 A CN201810653960 A CN 201810653960A CN 108558268 A CN108558268 A CN 108558268A
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- high temperature
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- temperature resistant
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/12—Condensation polymers of aldehydes or ketones
- C04B26/122—Phenol-formaldehyde condensation polymers
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/76—Use at unusual temperatures, e.g. sub-zero
- C04B2111/763—High temperatures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of fibre reinforced high temperature resistant adhesives and preparation method thereof, including：Adhering resin, reinforced phase, solid packing, curing agent；The adhering resin is phenolic resin, and reinforced phase is chopped carbon fiber, and solid packing is powdery B4C、SiO2, Si, curing agent is hexamethylenetetramine；Compare phenolic resin according to quality：Carbon fiber：B4C：SiO2：Si：Hexamethylenetetramine=100:1:50:10:2:10.The carbon fiber that the present invention uses, quality is lighter than metallic aluminium, but intensity is higher than steel, and has corrosion-resistant, high-modulus characteristic；, carbon yield high, thermostabilization good, at low cost the features such as various using phenolic resin structure, on the basis of filler is added in phenolic resin, after high-temperature process, phenolic resin decomposes charing and forms porous structure, due to the filling of high temperature resistant filler and the bridge linking effect of carbon fiber, it can make bonded joint that there is higher strength retention at high temperature.
Description
Technical field
The invention belongs to adhesive techniques field more particularly to a kind of fibre reinforced high temperature resistant adhesive and its preparation sides
Method.
Background technology
With the progress and development of science and technology, the structural member being operated in hot environment gradually increases, high temperature resistant bonding
The application demand of the application of agent is more and more wider.Especially led in some high-tech such as aerospace, mechanical chemical industry and automotive electronics
Domain, reliable high temperature adhesive are to realize the connection of complex structural member, and simplify preparation process, the key of reduction production cost.
Such as hypersonic aircraft due to flying speed it is fast, have huge military value and potential economic value, be each Air China
The important developing direction in empty field.When aircraft is with hypersonic speed flight in an atmosphere, Aerodynamic Heating is serious.Work as flying speed
When reaching 8 Mach, for the nose cone spot temperature of aircraft up to 1800 DEG C, the temperature at other positions also will be at 600 DEG C or more.Therefore
The selection of heat-resisting material, the design of thermal protection system and the exploitation of high temperature resistant adhesive are all the key that its development and application skills
Art.Also spaceship will be subjected to high temperature gas flow and wash away, surface temperature is needed up to 2300-2600 DEG C when reentrying
Heat-Resisting Adhesive is used for the bonding of ceramic insulation tile.For another example charcoal/charcoal (C/C) composite material is that most widely used aviation is stopped at present
Vehicle material.Since charcoal/carbon/carbon brake disc is consumable part, and it is expensive, the reparation of charcoal disk has significant economic implications.Mesh
Before, simple " two-in-one " adhering method of reparation generally use of charcoal disk.In view of aircraft braking disk with composite carbon/carbon material is tight
Transient temperature rise of bringing to a halt is more than 1000 DEG C, and reliable high temperature adhesive is the key that charcoal disk reparation.In addition, the zero of many spacecrafts
Component, in the preparation of clutch, sealing ring and the wearing piece applied in automobile, tank, panzer high temperature resistant adhesive be also must
One of raw material wanted.
Existing high temperature adhesive preparation process is complicated, and production cost is higher.
Invention content
The purpose of the present invention is to provide a kind of fibre reinforced high temperature resistant adhesives and preparation method thereof, it is intended to solve existing
Some high temperature adhesive preparation processes are complicated, the problem that production cost is higher, of less types.
The invention is realized in this way a kind of preparation method of fibre reinforced high temperature resistant adhesive, the carbon fiber increases
The preparation method of strong high temperature resistant adhesive includes the following steps：
(1) weigh 100 parts of phenolic resin respectively, 10 parts of hexamethylenetetramine, sequentially add be placed with appropriate absolute ethyl alcohol and
It is sufficiently stirred 10min with glass bar in the stirring vessel of hydroxypropyl methyl cellulose (HPMC) dispersant, keeps dispersant fully molten
It solves and is uniformly mixed.
(2) it is gradually added into chopped carbon fiber (average length<1mm) 1 part, pre-dispersed 10min is stirred with glass bar, then will stir
It mixes vessel to be placed in aqueous solution, decentralized processing 10min is carried out using the ultrasonic wave of 20kHz fixed frequencies.
(3) B is continuously added450 parts of C powder, SiO210 parts of powder, 2 parts of Si powder, is handled by ultrasonic activation, and is assisted with glass
Glass stick intermittent stirring 30min makes carbon fiber disperse abundant, each component and is uniformly mixed, obtains more sticky bonding agent.
Another object of the present invention is to provide a kind of preparations of the preparation method of fibre reinforced high temperature resistant adhesive
Fibre reinforced high temperature resistant adhesive, the fibre reinforced high temperature resistant adhesive includes：Adhering resin, reinforced phase, solid
Filler, curing agent；
The adhering resin is phenolic resin, and reinforced phase is chopped carbon fiber, and solid packing is powdery B4C、SiO2, Si, Gu
Agent is hexamethylenetetramine；
Compare phenolic resin according to quality：Carbon fiber：B4C：SiO2：Si：Hexamethylenetetramine=100:1:50:10:2:10.
The bonding agent obtained using this technical solution can be used as high temperature adhesive for graphite, ceramics, high molecular material
With the connection of the multiple materials such as carbon fibre reinforced composite, easy to operation, connector robust, performance are stablized, can
High temperature (being not higher than 1200 DEG C) working environment is born, is subjected to after high temperature that still there is good strength retention.
Another object of the present invention is to provide a kind of preparation methods using the fibre reinforced high temperature resistant adhesive
The bonding of the carbon/carbon composite of the fibre reinforced high temperature resistant adhesive of preparation.
Further, the bonding of the carbon/carbon composite includes the following steps：
Carbon/carbon composite is cut into fritter, it is spare after 95% EtOH Sonicate cleaning, to carbon/carbon compound material
Sample carries out surface polishing, uses the sand paper that granularity is 200# and 400# to polish successively, after being rinsed with clear water, is put into anhydrous second
It is cleaned by ultrasonic in alcohol, electricity consumption blowing drying is put into baking oven and is dried；
Bonding agent is coated uniformly on respectively on two pieces of C/C composite material surfaces by polishing cleaning, then by two pieces
C/C composite samples stick together be put into air dry oven make bonding agent carry out solidification C/C composite joints are made.
Another object of the present invention is to provide a kind of preparation methods using the fibre reinforced high temperature resistant adhesive
The fibre reinforced high temperature resistant adhesive of preparation and ceramics bondings.
Further, the method for the bonding of the ceramics includes the following steps：
Ceramics are cut into fritter, it is spare after 95% EtOH Sonicate cleaning, surface polishing is carried out to ceramic sample, according to
It is secondary to be polished using the sand paper that granularity is 200# and 400#, it after being rinsed with clear water, is put into absolute ethyl alcohol and is cleaned by ultrasonic, use
Hair dryer dries up, and is put into baking oven and is dried；
Bonding agent is coated uniformly on respectively on two pieces of ceramic surfaces by polishing cleaning, then by two pieces of ceramic samples
Stick together be put into air dry oven make bonding agent carry out solidification ceramic joint is made.
Fibre reinforced high temperature resistant adhesive provided by the invention and preparation method thereof, the carbon fiber (carbon used
Fiber, abbreviation CF), it is high intensity, the new fiber materials of high modulus fibre of a kind of phosphorus content 95% or more, is by piece
The organic fibers such as shape graphite microcrystal are piled up along fiber axial direction, through micro crystal graphite obtained from carbonization and graphitization processing
Material；Carbon fiber " soft outside but hard inside ", quality is lighter than metallic aluminium, but intensity is higher than steel, and with corrosion-resistant, high-modulus
Characteristic is all important materials in defence and military and civilian aspect.It not only has the intrinsic intrinsic property of carbon material, and has both spinning
The soft machinability of textured fiber is reinforcing fiber of new generation；It is various using phenolic resin structure, carbon yield is high, thermostabilization is good,
Some B are added in the features such as at low cost in phenolic resin4C、SiO2On the basis of Si fillers, after high-temperature process, phenolic aldehyde tree
Fat decomposes charing and forms porous structure, due to B4C、SiO2It, can be with the bridge linking effect of the filling and carbon fiber of Si high temperature resistant fillers
Make bonded joint that there is higher strength retention at high temperature.
Prepared fibre reinforced high temperature resistant adhesive the experiment proved that, it is made when being connected for C/C composite materials
Standby C/C composite materials bonded joint shear strength average out to 6.74MPa at room temperature.After 1200 DEG C are heat-treated 2h, connector
Shear strength is declined slightly, average value 5.34MPa.As heat treatment temperature is increased to 1400 DEG C, after keeping the temperature 2h, joints shear
Intensity is remarkably decreased, average value 1.48MPa.Illustrate, this high temperature adhesive can carry out work in the environment not higher than 1200 DEG C
Make, and with good performance.
Description of the drawings
Fig. 1 is the preparation method flow chart of fibre reinforced high temperature resistant adhesive provided in an embodiment of the present invention.
Fig. 2 is C/C composite materials technique for sticking flow chart provided in an embodiment of the present invention.
Fig. 3 is curing process heating curve schematic diagram provided in an embodiment of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
The fibre reinforced high temperature resistant adhesive of the embodiment of the present invention includes：Adhering resin, solid packing, is consolidated reinforced phase
Agent.
Adhering resin is phenolic resin, and reinforced phase is mainly chopped carbon fiber, and solid packing is powdery B4C、SiO2, Si, Gu
Agent is hexamethylenetetramine.
Compare phenolic resin according to quality：Carbon fiber：B4C：SiO2：Si：Hexamethylenetetramine=100:1:50:10:2:10.
The bonding agent of the present invention is mainly used in the bonding of carbon/carbon composite and ceramics etc..
As shown in Figure 1, the preparation method of the fibre reinforced high temperature resistant adhesive of the embodiment of the present invention includes the following steps：
(1) weigh 100 parts of phenolic resin respectively, 10 parts of hexamethylenetetramine, sequentially add be placed with appropriate absolute ethyl alcohol and
It is sufficiently stirred 10min with glass bar in the stirring vessel of hydroxypropyl methyl cellulose (HPMC) dispersant, keeps dispersant fully molten
It solves and is uniformly mixed.
(2) it is gradually added into chopped carbon fiber (average length<1mm) 1 part, pre-dispersed 10min is stirred with glass bar, then will stir
It mixes vessel to be placed in aqueous solution, decentralized processing 10min is carried out using the ultrasonic wave of 20kHz fixed frequencies.
(3) B is continuously added450 parts of C powder, SiO210 parts of powder, 2 parts of Si powder, is handled by ultrasonic activation, and is assisted with glass
Glass stick intermittent stirring 30min makes carbon fiber disperse abundant, each component and is uniformly mixed, obtains more sticky bonding agent.
The application effect of the present invention is explained in detail with reference to experiment.
Implementation process：C/C composite materials are cut into 30mm × 20mm × 4mm3Fritter, it is clear through 95% EtOH Sonicate
It washes rear spare.Before experiment, surface polishing is carried out to carbon/carbon compound material sample, it is the sand of 200# and 400# to use granularity successively
Paper, polishing every time will be handled specimen surface consistent to finish, smooth to surface along direction uniform grinding of exerting oneself,
The abrasive dust for removing surface simultaneously, after being rinsed with clear water, is put into absolute ethyl alcohol and is cleaned by ultrasonic (30min or so), electricity consumption
Blowing drying, is put into baking oven and is dried.
By according to the fibre reinforced high temperature resistant adhesive shown in Fig. 1 and prepared by the above method be coated uniformly on respectively through
It crosses on two pieces of C/C composite material surfaces of polishing cleaning, then two pieces of C/C composite samples, which stick together, is put into air blast and does
Dry case make bonding agent carry out solidification C/C composite joints are made.C/C composite material technique for sticking flow charts and curing process liter
Warm curve synoptic diagram difference is as shown in Figures 2 and 3.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (6)
1. a kind of preparation method of fibre reinforced high temperature resistant adhesive, which is characterized in that the fibre reinforced high temperature resistant is viscous
The preparation method for connecing agent includes the following steps：
(1) 100 parts of phenolic resin is weighed respectively, and 10 parts of hexamethylenetetramine sequentially adds and is placed with appropriate absolute ethyl alcohol and hydroxypropyl
It is sufficiently stirred 10min with glass bar in the stirring vessel of ylmethyl cellulose dispersant, dispersant is made fully to dissolve and is mixed
It is even；
(2) it is gradually added into 1 part of chopped carbon fiber, stirs pre-dispersed 10min with glass bar, then stirring vessel are placed in aqueous solution
In, decentralized processing 10min is carried out using the ultrasonic wave of 20kHz fixed frequencies；
(3) B is continuously added450 parts of C powder, SiO210 parts of powder, 2 parts of Si powder, is handled by ultrasonic activation, and is assisted with glass bar
Intermittent stirring 30min makes carbon fiber disperse abundant, each component and is uniformly mixed, obtains bonding agent.
2. the resistance to height of fibre reinforced prepared by a kind of preparation method of fibre reinforced high temperature resistant adhesive as described in claim 1
Warm bonding agent, which is characterized in that the fibre reinforced high temperature resistant adhesive includes：Adhering resin, reinforced phase, solid packing,
Curing agent；
The adhering resin is phenolic resin, and reinforced phase is chopped carbon fiber, and solid packing is powdery B4C、SiO2, Si, curing agent
For hexamethylenetetramine；
Compare phenolic resin according to quality：Carbon fiber：B4C：SiO2：Si：Hexamethylenetetramine=100:1:50:10:2:10.
3. fibre reinforced prepared by a kind of preparation method using fibre reinforced high temperature resistant adhesive described in claim 1 is resistance to
The bonding of the carbon/carbon composite of high temperature adhesive.
4. the bonding of carbon/carbon composite as claimed in claim 3, which is characterized in that the bonding of the carbon/carbon composite
Include the following steps：
Carbon/carbon composite is cut into fritter, it is spare after 95% EtOH Sonicate cleaning, to carbon/carbon compound material sample
Surface polishing is carried out, uses the sand paper that granularity is 200# and 400# to polish successively, after being rinsed with clear water, is put into absolute ethyl alcohol
It is cleaned by ultrasonic, electricity consumption blowing drying is put into baking oven and is dried；
Bonding agent is coated uniformly on respectively on two pieces of C/C composite material surfaces by polishing cleaning, then answers two pieces of C/C
Condensation material sample stick together be put into air dry oven make bonding agent carry out solidification C/C composite joints are made.
5. fibre reinforced prepared by a kind of preparation method using fibre reinforced high temperature resistant adhesive described in claim 1 is resistance to
The bonding of the ceramics of high temperature adhesive.
6. a kind of method of the bonding of ceramics as claimed in claim 5, which is characterized in that the method packet of the bonding of the ceramics
Include following steps：
Ceramics are cut into fritter, it is spare after 95% EtOH Sonicate cleaning, surface polishing is carried out to ceramic sample, is made successively
It is 200# and the polishing of the sand paper of 400# with granularity, after being rinsed with clear water, is put into absolute ethyl alcohol and is cleaned by ultrasonic, electricity consumption is blown
Wind is dry, is put into baking oven and is dried；
Bonding agent is coated uniformly on respectively on two pieces of ceramic surfaces by polishing cleaning, is then sticked to two pieces of ceramic samples
Be put into togerther air dry oven make bonding agent carry out solidification ceramic joint is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810653960.6A CN108558268A (en) | 2018-06-22 | 2018-06-22 | A kind of fibre reinforced high temperature resistant adhesive and preparation method thereof |
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| CN201810653960.6A CN108558268A (en) | 2018-06-22 | 2018-06-22 | A kind of fibre reinforced high temperature resistant adhesive and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909532A (en) * | 2020-08-14 | 2020-11-10 | 长沙创远环保科技有限公司 | Environment-friendly flame-retardant straw board for building and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN103755375A (en) * | 2014-02-12 | 2014-04-30 | 鞍山塞诺达碳纤维有限公司 | Binding agent used for carbon materials in high-temperature furnace and application method |
| CN104974697A (en) * | 2015-07-21 | 2015-10-14 | 中国科学院上海应用物理研究所 | Carbon/carbon composite material binder, bonding method and carbon/carbon composite material member |
-
2018
- 2018-06-22 CN CN201810653960.6A patent/CN108558268A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755375A (en) * | 2014-02-12 | 2014-04-30 | 鞍山塞诺达碳纤维有限公司 | Binding agent used for carbon materials in high-temperature furnace and application method |
| CN104974697A (en) * | 2015-07-21 | 2015-10-14 | 中国科学院上海应用物理研究所 | Carbon/carbon composite material binder, bonding method and carbon/carbon composite material member |
Non-Patent Citations (2)
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| 乔吉超等: "酚醛树脂胶粘剂的研究进展", 《中国胶粘剂》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909532A (en) * | 2020-08-14 | 2020-11-10 | 长沙创远环保科技有限公司 | Environment-friendly flame-retardant straw board for building and preparation method thereof |
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