CN106147676A - A kind of preparation method of silicon carbide whisker silica filled organopolysiloxane resin high temperature adhesive - Google Patents
A kind of preparation method of silicon carbide whisker silica filled organopolysiloxane resin high temperature adhesive Download PDFInfo
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- CN106147676A CN106147676A CN201510162967.4A CN201510162967A CN106147676A CN 106147676 A CN106147676 A CN 106147676A CN 201510162967 A CN201510162967 A CN 201510162967A CN 106147676 A CN106147676 A CN 106147676A
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- silicon carbide
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- high temperature
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- whisker
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Abstract
Prepared by a kind of exotic material high temperature resistant adhesive, it is characterised in that preparation process is divided into four: step one: it is stirring 30min in 5% ethanol solution that inorganic filler is put into silane coupled agent content, dries.Step 2: silicon carbide whisker in the acetone solvent containing 5%KH550, ultrasonic disperse 2h.Step 3: use the silane coupled coupling under the conditions of 80-95 DEG C by epoxy and organic siliconresin.Filler, whisker, resin are mixed by a certain percentage.Step 4: bonding agent is coated uniformly in the middle of two sheet materials that will be bonding, takes the mode of the changing of the relative positions to bond together, and uses fixing device fixed plate, 72h solidification under the conditions of room temperature (25 DEG C).It is proven: the material after bonding, under the conditions of 1200 DEG C, still has good mechanical property.Bonding agent thermal weight loss rate prepared by the present invention is low, acid-proof alkaline is excellent, has practical value and application widely in the bonding field of exotic material.
Description
Technical field
The present invention relates to high temperature adhesive Material Field, particularly to a kind of preparation method being applicable to exotic material bonding agent.
Background technology
Ceramic material, carbon carbon composite have been widely used in the multinomial fields such as Aero-Space as exotic material.Owing to Aero-Space device structure is complicated, in an assembling process, it is usually present fragility big, is difficult to multiple difficulties such as one-body molded, in order to preferably reach using effect, in different ceramic components connect, have employed bonding combination.
When bonding high temperature resistant component, in order to enable preferably to make adhering part fasten, when using in high temperature environments, still higher mechanical strength can be kept, make bonding high temperature resistant component still can use, be unlikely to because bonding site performance is undesirable, and affect the performance of whole device.Under these conditions, the bonding agent for bonding exotic material just proposes the highest requirement, it is desirable to it had both been amenable to the test of hot environment, meanwhile, the fastening adhesion effect of bonding agent to be played own, and kept good mechanical property.
At present, the bonding agent of domestic and international exotic material is broadly divided into two types, respectively inorganic high-temperature resistant bonding agent and organic high temperature-resistant bonding agent.Inorganic type high temperature resistant adhesive mainly has phosphate base high temperature resistant adhesive and nitrate-based high temperature resistant adhesive.The shortcomings such as inorganic type high temperature resistant adhesive heat resistance is excellent, is amenable to the high temperature of 2000-3000 DEG C, but it is big to there is also fragility, poor ductility, easy moisture absorption.Organic type high temperature resistant adhesive mainly has the high temperature resistant adhesive of the types such as silicone, phenolic, amide-type, the mechanical strength of organic type high temperature resistant adhesive is preferable, there are higher specific strength and specific modulus, but there is the shortcomings such as heat resistance is poor, constrain its application in superhigh temperature field.
Summary of the invention
1. goal of the invention: in order to better meet the bonding requirements of exotic material, obtains using in high temperature environments, meanwhile, and higher adhesive strength so that the exotic material parts of bonding agent can use in high temperature environments and not affect its mechanical strength.
2. technical scheme: the present invention is prepared by a kind of exotic material bonding agent, it is characterised in that: the bonding agent that exotic material uses mainly can complete construction under cryogenic, uses under the high temperature conditions.Its preparation method is as follows:
Step one: filling surface processes.Take a certain amount of dehydrated alcohol, it is added to silane coupler in the ratio of 5%, after being uniformly mixed, add the inorganic filler of equivalent, mechanical agitation 30min, put in ultrasonic disperse machine, ultrasonic disperse 1h, after taking-up, is placed in 100 DEG C of baking ovens drying by inorganic filler, take in after drying in valve bag, for later.
Step 2: whisker surface processes.Use commercial grade silicon carbide whisker, be immersed in the acetone solvent containing 5%KH550, soak 2h.Use churned mechanically mode, stir 2h.Ultrasonic disperse, ultrasonic disperse 3h is carried out to through modified silicon carbide whisker.
Step 3: major ingredient is prepared.Use herein and silane coupled epoxy resin and organic siliconresin are carried out coupling under the conditions of uniform temperature, be prepared for the major ingredient resin of high temperature resistant adhesive.Bonding agent major ingredient and the most surface-treated silicon carbide whisker solution are mixed, uses the mode of rotary evaporation, remove acetone solvent therein.After solvent is evaporated, the bonding agent major ingredient of containing silicon carbide whisker is mixed homogeneously in 5:5 ratio with filler, add firming agent Versamid 650 and catalyst dibutyltin dilaurylate.Use the mode mix homogeneously of stirring.
Step 4: adhering method.The adhesives processed is positioned on smooth desktop, uses little scraper to touch and take the bonding agent that a small amount of hybrid process is good, be coated uniformly on will be bonding two sheet materials in the middle of, with scraper, gluing of surfaces is struck off, two sheet materials are taked the mode of the changing of the relative positions, bonds to one piece, the changing of the relative positions repeatedly, drive bubble in adhesive linkage away, use fixing device is by two sheet material fix tightlies, and applies certain pressure, is placed on 72h in room temperature (25 DEG C) environment, after taking-up, obtain bonding ceramic material.
Being epoxy resin E-51 according to the epoxy resin described in claims 1, the organic siliconresin of use is methyl phenyl silicone resin.
It is mainly Al powder (200-300 mesh), ZrO according to the inorganic filler described in claims 12Powder (200-300 mesh), B4C powder (100-200 mesh).
The churned mechanically time is used to be 15min according to the inorganic filler described in claims 1, organic major ingredient, whisker.
It is 70-100 DEG C according to the epoxy resin described in claims 1 and organic siliconresin coupling temperature.
3. having an advantage in that the preparation process that the present invention relates to a kind of exotic material bonding agent, main use temperature is 700-1200 DEG C.Use this bonding agent, can the most bonding construction, place after 72h and can be fully cured, reach to use requirement.High temperature resistant component after bonding is placed in hot environment use, still can keep high mechanical strength, play good adhesive effect.
(1) present invention is under the high temperature conditions, excellent in mechanical performance, and in high temperature environments, after experiencing 1000 DEG C of calcining 2h, shear strength still can reach 20MPa
(2) thermal weight loss rate of the present invention is low, after experience uses thermogravimetic analysis (TGA), draws after 900 DEG C of calcinations, and weight-loss ratio is 43.2%
(3) solidification temperature of the present invention is low, after placing 72h at 25 DEG C, through infrared analysis, finds that bonding agent has cured, and Sticking condition is gentle, and construction easily realizes.
(4) present invention is acidproof and alkaline resistance properties excellent, and after soaking 30 days in 10%H2SO4 and 10%NaOH solution, quality only loss of weight is only 3.1% and 4.8%.
(5) present invention has certain toughness, at the standard batten of preparation, after using GB GB/T 6569-2006 to test, finds that its bending strength is 26.83MPa excellent performance.
(4) accompanying drawing explanation
The enforcement operational flowchart of Fig. 1 present invention
Fig. 2 major ingredient of the present invention, filler preparation process figure
Fig. 3 bonding agent inner scanning ultramicroscope picture
Fig. 4 bonding agent thermogravimetric curve figure
Fig. 5 bonding agent corrosion resistance: time m-mass change figure
(5) detailed description of the invention
Example 1
Alumina ceramic plate bonding.
Step one: take the alumina ceramic plate two panels of same size, cleans with acetone, then dries 2h under the conditions of 150 DEG C, takes out standby.Step 2: filling surface processes.Take 20ml dehydrated alcohol, it is added to Silane coupling agent KH550 in the ratio of 5%, after being uniformly mixed, add the boron carbide of 3g, mechanical agitation 30min, put in ultrasonic disperse machine, ultrasonic disperse 1h, after taking-up, is placed in 100 DEG C of baking ovens drying by inorganic filler, take in valve bag after drying, in case use later.
Step 3: whisker surface processes.Weigh silicon carbide whisker 0.2g, be immersed in the acetone solvent containing 5%KH550, soak 2h.Use churned mechanically mode, stir 2h.Ultrasonic disperse, ultrasonic disperse 3h is carried out to through modified silicon carbide whisker.
Step 3: major ingredient is prepared.Using silane coupled KH560 that epoxy resin (E-51) and organic siliconresin are carried out under the conditions of 85 DEG C mechanical agitation mixing herein, the response time is 1h.Bonding agent major ingredient and the most surface-treated silicon carbide whisker solution are mixed, uses the mode of rotary evaporation, remove acetone solvent therein.After solvent is evaporated, the bonding agent major ingredient of containing silicon carbide whisker is mixed homogeneously in 5:5 ratio with filler, add firming agent Versamid 651 and catalyst dibutyltin dilaurylate.Use the mode mix homogeneously of stirring.
Step 4: adhering method.The adhesives processed is positioned on smooth desktop, uses the bonding agent that the little a small amount of hybrid process of scraper picking is good, be coated uniformly on will be bonding alumina ceramic plate surface, coated area is the 1/2 of aluminium oxide ceramics plate plane.With scraper, gluing of surfaces is struck off, mode the two panels aluminium oxide ceramics piece collection changing of the relative positions, bond to one piece, the changing of the relative positions repeatedly, drives bubble in adhesive linkage away, uses fixing device to be fixed by alumina ceramic plate, and apply certain pressure, it is placed on 72h in room temperature (25 DEG C) environment, after taking-up, obtains bonding aluminium oxide ceramics sheet material.
Claims (5)
1. the present invention is prepared by a kind of silicon carbide whisker silica filled organopolysiloxane resin high temperature resistant adhesive, its
It is characterised by: use bonding agent in the present invention can complete construction under cryogenic, at height
Use under the conditions of temperature.Its preparation method is as follows:
Step one: filling surface processes.Take a certain amount of dehydrated alcohol, add wherein in the ratio of 5%
Add silane coupler, after being uniformly mixed, add the inorganic filler of equivalent, mechanical agitation
30min, puts into ultrasonic disperse 1h in ultrasonic disperse machine, after taking-up, inorganic filler is put
Put and dry in 100 DEG C of baking ovens, take in after drying in valve bag, for later.
Step 2: whisker surface processes.Use commercial grade silicon carbide whisker, be immersed in containing
In the acetone solvent of 5%KH550, soak 2h.Use churned mechanically mode, stirring
2h.Ultrasonic disperse, ultrasonic disperse 3h is carried out to through modified silicon carbide whisker.
Step 3: major ingredient is prepared.Use herein and silane coupled epoxy resin and organic siliconresin are existed
Carry out coupling under the conditions of uniform temperature, be prepared for the major ingredient resin of high temperature resistant adhesive.Will be viscous
Connect agent major ingredient and the mixing of the most surface-treated silicon carbide whisker solution, use the side of rotary evaporation
Formula, removes acetone solvent therein.After solvent is evaporated, gluing containing silicon carbide whisker
Connect agent major ingredient to mix homogeneously in 5:5 ratio with filler, add firming agent Versamid 650
With catalyst dibutyltin dilaurylate.Use the mode mix homogeneously of stirring.
Step 4: adhering method.The adhesives processed is positioned on smooth desktop, uses
Little scraper is touched and is taken the bonding agent that a small amount of hybrid process is good, be coated uniformly on will be bonding two panels
In the middle of sheet material, with scraper, gluing of surfaces is struck off, two sheet materials is taked the mode of the changing of the relative positions,
Bond to one piece, the changing of the relative positions repeatedly, drive bubble in adhesive linkage away, use fixing device by two panels
Sheet material fix tightly, and apply certain pressure, it is placed in room temperature (25 DEG C) environment
72h, after taking-up, waits high-temperature process.
2. it is epoxy resin E-51 according to the epoxy resin described in claims 1, having of use
Machine silicones is methyl phenyl silicone resin.
3. according to the inorganic filler described in claims 1 be mainly Al powder (200-300 mesh),
ZrO2Powder (200-300 mesh), B4C powder (100-200 mesh).
4. use machinery according to the inorganic filler described in claims 1, organic major ingredient, whisker
The time of stirring is 15min.
5. it is 70-according to the epoxy resin described in claims 1 and organic siliconresin coupling temperature
100℃。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510162967.4A CN106147676A (en) | 2015-04-08 | 2015-04-08 | A kind of preparation method of silicon carbide whisker silica filled organopolysiloxane resin high temperature adhesive |
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| CN201510162967.4A CN106147676A (en) | 2015-04-08 | 2015-04-08 | A kind of preparation method of silicon carbide whisker silica filled organopolysiloxane resin high temperature adhesive |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439212A (en) * | 2018-11-07 | 2019-03-08 | 合肥凯大新型材料科技有限公司 | A kind of carbon/carbon compound material low bulk adhesive |
| CN109880500A (en) * | 2019-01-28 | 2019-06-14 | 南京林业大学 | The preparation method of nano boron carbide modified aqueous polyurethane high wear resistance coatings |
| CN111171779A (en) * | 2018-11-11 | 2020-05-19 | 天津大学青岛海洋技术研究院 | Preparation method of wide-temperature-range high-temperature-resistant composite adhesive |
| CN113174206A (en) * | 2021-06-04 | 2021-07-27 | 成都工业学院 | High-temperature-resistant high-strength ceramic high-temperature glue, and preparation method and application thereof |
-
2015
- 2015-04-08 CN CN201510162967.4A patent/CN106147676A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439212A (en) * | 2018-11-07 | 2019-03-08 | 合肥凯大新型材料科技有限公司 | A kind of carbon/carbon compound material low bulk adhesive |
| CN111171779A (en) * | 2018-11-11 | 2020-05-19 | 天津大学青岛海洋技术研究院 | Preparation method of wide-temperature-range high-temperature-resistant composite adhesive |
| CN109880500A (en) * | 2019-01-28 | 2019-06-14 | 南京林业大学 | The preparation method of nano boron carbide modified aqueous polyurethane high wear resistance coatings |
| CN113174206A (en) * | 2021-06-04 | 2021-07-27 | 成都工业学院 | High-temperature-resistant high-strength ceramic high-temperature glue, and preparation method and application thereof |
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