CN104861884A - Method for bonding carbon fiber/phenolic-nitrile rubber materials - Google Patents

Method for bonding carbon fiber/phenolic-nitrile rubber materials Download PDF

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Publication number
CN104861884A
CN104861884A CN201510247734.4A CN201510247734A CN104861884A CN 104861884 A CN104861884 A CN 104861884A CN 201510247734 A CN201510247734 A CN 201510247734A CN 104861884 A CN104861884 A CN 104861884A
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thermal insulation
ethylene propylene
carbon fiber
propylene terpolymer
nitrile rubber
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CN104861884B (en
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崔瑞禧
吕春祥
朱稼麟
杨禹
宋考生
张颖新
邓安华
陈丽萍
王凯
刘后浪
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Shanxi Institute of Coal Chemistry of CAS
Hubei Sanjiang Aerospace Jianghe Chemical Technology Co Ltd
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Shanxi Institute of Coal Chemistry of CAS
Hubei Sanjiang Aerospace Jianghe Chemical Technology Co Ltd
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Abstract

The invention discloses a method for bonding carbon fiber/phenolic-nitrile rubber materials, and belongs to the field of the manufacturing of a solid rocket engine insulator, and aims at solving the bonding problems of an engine housing, a first EPDM insulation material, a carbon fiber/phenolic-nitrile rubber materials and a second EPDM insulation material and improving the structural reliability. The method mainly comprises the steps of preparation, coating, prefabrication, cleaning, glue coating, setting, thermal pre-pressing, flaw detection, curing and the like. The structural integrity of the engine housing, a first EPDM insulation material, the carbon fiber/phenolic-nitrile rubber materials and the second EPDM insulation material are ensured by using a secondary bonding method, a secondary curing mode, a prefabrication forming method, a stepped temperature rising/dropping mode and other methods; the method has no de-bonding, air-entraining air hole and other quality problems, completely can meet the design requirements, and ensures the safety and reliability of a system.

Description

A kind of adhering method of carbon fiber/phenolic aldehyde-nitrile rubber
Technical field
The invention belongs to solid propellant rocket thermal insulation layer manufacture method, be specifically related to a kind of adhering method of carbon fiber/phenolic aldehyde-nitrile rubber.
Background technology
Carbon fiber/phenolic aldehyde-nitrile rubber is a kind of matrix material by obtaining after paracril, impregnated carbon fiber resol, has excellent heat-insulating property and application prospect widely.This material hardness is large, unit elongation is lower, not easily discharge stress, therefore, in engine research, development process, devise the structural pattern of motor body, Ethylene Propylene Terpolymer thermal insulation material (bottom)/carbon fiber/phenolic aldehyde-nitrile rubber/Ethylene Propylene Terpolymer thermal insulation material (surface layer), adopt chemical adhesive to complete the effective connection between material, by using the elastomeric thermal insulation material that has that terpolymer EP rubber is matrix to discharge stress, thus obtain good net effect.This structural interface is many, and material property is different, and it is very difficult for effectively connecting.Simultaneously, carbon fiber/phenolic aldehyde-nitrile rubber contains moisture content and the solvent of trace, its phenolic component, a certain amount of micro-molecular gas can be produced during solidification, cleaning and tackiness agent use the remaining of solvent, thus there will be the quality problems such as unsticking, interlayer gas enclosure, especially when thickness is larger, problem is particularly serious.
Summary of the invention
The invention provides a kind of adhering method of carbon fiber/phenolic aldehyde-nitrile rubber, solve the bonding difficult problem between motor body, Ethylene Propylene Terpolymer thermal insulation material (bottom), carbon fiber/phenolic aldehyde-nitrile rubber, Ethylene Propylene Terpolymer thermal insulation material (surface layer), improve its reliability of structure.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of adhering method of carbon fiber/phenolic aldehyde-nitrile rubber, comprise motor body bonding successively, Ethylene Propylene Terpolymer thermal insulation of materials material, carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials material, its concrete bonding step is:
1) preliminary step: according to engine insulating structure dimensional requirement, by Ethylene Propylene Terpolymer thermal insulation material roller-compaction, by shaping for carbon fiber/phenolic aldehyde-nitrile rubber cutting; When there is end socket position, adopt mould compression molding;
2) squeegeeing step: carbon fiber/phenolic aldehyde-nitrile rubber is cleaned out, hangs 1 ~ 2h; Brushing CH238 tackiness agent, adhesive glue film gauge control, at 5 μm ~ 10 μm, hangs 1 ~ 2h or takes air blast or heating measures; Ethylene Propylene Terpolymer thermal insulation of materials material is cleaned out, and hangs 1 ~ 2h; Brushing CH238 glue, adhesive glue film gauge control, at 5 μm ~ 10 μm, hangs 1 ~ 2h or takes air blast or heating measures;
3) prefabrication step: by the carbon fiber/phenolic aldehyde-nitrile rubber after brushing adhesive stick and Ethylene Propylene Terpolymer thermal insulation of materials material to subsides; Put into vulcanizing press or pressure-pot carries out hot pressing, hot pressing pressure is 1MPa ~ 2MPa, and hot pressing temperature is 70 DEG C ~ 80 DEG C, and the heat-insulation pressure keeping time is 30min ~ 60min, period, decompression exhaust 2 ~ 3 times; After hot pressing terminates, be down to room temperature, take out prefabricated carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials combination of materials part;
4) cleanup step: motor body internal surface adopts the one in technical grade ethyl acetate, trichloromethane or acetone to clean out, and hangs 1 ~ 2h or takes air blast or heating measures;
5) brush coating step: motor body inner homogeneous brushing adhesive stick, tackiness agent is CH205, and adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h; Then brush CH238, adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h;
6) placing step: by 3) in the subassembly of gained put into motor body preposition, the one side of the Ethylene Propylene Terpolymer thermal insulation of materials material of subassembly is fitted with motor body, pressurizes with air or with Silicon rubber inflatable bag;
7) hot pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C ~ 100 DEG C, pressure 0.6MPa ~ 1.0MPa, heating, clamping time 1h ~ 3h, heat, pressurize complete, engine is taken out from heating unit;
8) flaw detection step: adopt digital ultrasonic flaw detector to Ethylene Propylene Terpolymer thermal insulation material and the flaw detection of motor body adhesion interface, check whether and occur unsticking phenomenon, be, go to step 8), otherwise order is carried out;
9) curing schedule: inserted by engine in heating unit, after pressurization, is warming up to 110 DEG C ± 5 DEG C, insulation 2h, and then temperature control rises to 165 DEG C ± 5 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 100 DEG C ± 5 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.1MPa ± 0.1MPa; Engine is taken out from heating unit;
10) cleaning step: the carbon fiber/phenolic aldehyde-nitrile rubber of the subassembly after solidification is cleaned, simultaneously to Ethylene Propylene Terpolymer material clean, hangs 1h ~ 2h or take air blast or heating measures;
11) glue application step: the carbon fiber/phenolic aldehyde-nitrile rubber one side of subassembly after hardening brushes CH238, and adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h;
12) secondary placing step: Ethylene Propylene Terpolymer thermal insulation of materials material is put into motor body preposition, Ethylene Propylene Terpolymer thermal insulation material and the carbon fiber/phenolic aldehyde-nitrile rubber be cured are fitted, and pressurize with air or with Silicon rubber inflatable bag;
13) second heat pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C ~ 100 DEG C, pressure 0.6MPa ~ 1.0MPa, heating, clamping time 1h ~ 3h, heat, pressurize complete, engine is taken out from heating unit;
14) step is checked: check whether Ethylene Propylene Terpolymer thermal insulation material surface occurs bubble, existence then adopts pinprick, tiltedly cuts mode degasification, then goes to step 13), otherwise carry out subsequent disposal;
15) regelate step: inserted by engine in heating unit, after being forced into 1.1MPa ± 0.1MPa, is warming up to 110 DEG C ± 5 DEG C, insulation 2h, and then temperature control rises to 165 DEG C ± 5 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 100 DEG C ± 5 DEG C again, and cooling rate is 15 DEG C/h, is finally down to room temperature, takes out engine and namely completes the bonding process of carbon fiber/phenolic aldehyde-nitrile rubber as thermal insulation material.
Described 2) squeegeeing step and 10) in cleaning step, adopt chemical pure ethyl acetate to carry out clean.
Described 2) squeegeeing step, 4) cleanup step and 10) in cleaning step, blasting time is 1 ~ 2h.
Described 2) squeegeeing step, 4) cleanup step and 10) in cleaning step, the temperature of heating measures is 50 DEG C ~ 60 DEG C, and the time is 1 ~ 2h.
Described 5) in brush coating step, while to motor body inner homogeneous brushing adhesive stick, brush CH238 in the Ethylene Propylene Terpolymer thermal insulation of materials material one side of subassembly, adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h.
Described 11), in glue application step, simultaneously at Ethylene Propylene Terpolymer thermal insulation of materials material brushing CH238, adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h.
The present invention adopts that secondary is bonding, regelate pattern, can progressively sequentially complete many materials, multiple solutions effectively bonding, avoid once the generation of the quality problems such as unsticking, pore, gas enclosure that bonding, one-step solidification pattern is easily formed; Adopt pre-formed method, end socket then adopts mould mold pressing can guarantee the anastomose property with motor body profile, can get rid of by decompression exhaust the gas that material, tackiness agent and operation produce, can guarantee effectively to fit between Ethylene Propylene Terpolymer thermal insulation material, carbon fiber/phenolic aldehyde-nitrile rubber; Adopt the pattern of two-sided brushing adhesive stick, tackiness agent can be made effectively can to infiltrate bonding plane, thus improve bonding strength further; The best curing temperature of various material and tackiness agent is different, staged heats up and cooling mode can make various material and tackiness agent effectively be solidified, meanwhile, the thermal stresses that material and bonding plane produce in the curing process can be eliminated, avoid thermal stresses to cause interfacial detachment.
This adhering method is the multiple product of successful Application.Product is all crowned with complete success through ground experiment.Thermal insulation layer dissection and analysis after test, structural integrity between motor body, Ethylene Propylene Terpolymer thermal insulation material (bottom), carbon fiber/phenolic aldehyde-nitrile rubber, Ethylene Propylene Terpolymer thermal insulation material (surface layer), without quality problems such as unsticking, gas enclosure pores, can meet design requirement completely, ensure that the safety and reliability of system.
Accompanying drawing explanation
Fig. 1 is engine after adopting method of the present invention bonding and the structure iron of thermal insulation layer.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope of embodiment statement.
By the engine insulating structure that obtains after the processing mode of embodiment as shown in Figure 1.Wherein 1 is motor body, and 2 is Ethylene Propylene Terpolymer thermal insulation material (bottom), and 3 is carbon fiber/phenolic aldehyde-nitrile rubber, and 4 is Ethylene Propylene Terpolymer thermal insulation material (surface layer).
Embodiment 1:
Certain solid propellant rocket, Ethylene Propylene Terpolymer thermal insulation material (bottom) 3mm is thick, and carbon fiber/phenolic aldehyde-nitrile rubber 6mm is thick, and Ethylene Propylene Terpolymer thermal insulation material (surface layer) 4mm is thick;
1) preliminary step: according to engine insulating structure dimensional requirement, by Ethylene Propylene Terpolymer thermal insulation material roller-compaction, by shaping for carbon fiber/phenolic aldehyde-nitrile rubber cutting;
2) squeegeeing step: adopt chemical pure ethyl acetate to clean out carbon fiber/phenolic aldehyde-nitrile rubber, hang 1h; Brushing CH238 glue, adhesive glue film gauge control, at 5 μm, hangs 1h; Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) adopts chemical pure ethyl acetate to clean out, and hangs 1h; Brushing CH238 glue, adhesive glue film gauge control, at 5 μm, hangs 1h;
3) prefabrication step: by the carbon fiber/phenolic aldehyde-nitrile rubber after brushing adhesive stick and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) to subsides; Put into vulcanizing press or pressure-pot carries out hot pressing, hot pressing pressure is 1MPa, and hot pressing temperature is 70 DEG C, and the heat-insulation pressure keeping time is 30min, period, can decompression exhaust 2 times; After hot pressing terminates, be down to room temperature, take out prefabricated carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) subassembly (abbreviation prefabricated component);
4) cleanup step: motor body internal surface adopts technical grade ethyl acetate to clean out, and hangs 1h;
5) brush coating step: motor body inner homogeneous brushing adhesive stick, tackiness agent is CH205, and adhesive glue film thickness is 5 μm, hangs 1h; Then brush CH238, adhesive glue film thickness is 5 μm, hangs 1h;
6) placing step: prefabricated component is put into motor body preposition, the one side of the Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) of prefabricated component is fitted with motor body, available air or pressurize with Silicon rubber inflatable bag;
7) hot pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C, pressure 0.6MPa, heating, clamping time 1h, heat, pressurize complete, engine is taken out from heating unit;
8) flaw detection step: adopt digital ultrasonic flaw detector to Ethylene Propylene Terpolymer thermal insulation material (bottom) and the flaw detection of motor body adhesion interface, without occurring unsticking phenomenon, order is carried out;
9) curing schedule: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 160 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit;
10) cleaning step: clean with the carbon fiber/phenolic aldehyde-nitrile rubber of chemical pure ethyl acetate to the prefabricated component after solidification, by chemical pure ethyl acetate, Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is cleaned, hang 1h;
11) glue application step: the carbon fiber/phenolic aldehyde-nitrile rubber one side of prefabricated component after hardening brushes CH238, and adhesive glue film thickness is 5 μm, hangs 1h;
12) secondary placing step: Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is put into motor body preposition, Ethylene Propylene Terpolymer thermal insulation material (surface layer) and the carbon fiber/phenolic aldehyde-nitrile rubber be cured are fitted, available air or pressurize with Silicon rubber inflatable bag;
13) second heat pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C, pressure 0.6MPa, heating, clamping time 1h, heat, pressurize complete, engine is taken out from heating unit;
14) check step: Ethylene Propylene Terpolymer thermal insulation material (surface layer) surperficial bubble-free, order is carried out;
15) regelate step: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 160 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit.
This product is all crowned with complete success through ground experiment.Thermal insulation layer dissection and analysis after test, structural integrity between motor body/Ethylene Propylene Terpolymer thermal insulation material (bottom)/carbon fiber/phenolic aldehyde-nitrile rubber/Ethylene Propylene Terpolymer thermal insulation material (surface layer), without quality problems such as unsticking, gas enclosure pores, can meet design requirement completely.
Embodiment 2:
Certain solid propellant rocket, Ethylene Propylene Terpolymer thermal insulation material (bottom) 2mm is thick, and carbon fiber/phenolic aldehyde-nitrile rubber 4mm is thick, and Ethylene Propylene Terpolymer thermal insulation material (surface layer) 4mm is thick;
1) preliminary step: according to engine insulating structure dimensional requirement, by Ethylene Propylene Terpolymer thermal insulation material roller-compaction, by shaping for carbon fiber/phenolic aldehyde-nitrile rubber cutting;
2) squeegeeing step: adopt chemical pure ethyl acetate to clean out carbon fiber/phenolic aldehyde-nitrile rubber, hang 1h; Brushing CH238 glue, adhesive glue film gauge control, at 10 μm, hangs 2h; Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) adopts chemical pure ethyl acetate to clean out, and hangs 1h; Brushing CH238 glue, adhesive glue film gauge control, at 10 μm, hangs 2h;
3) prefabrication step: by the carbon fiber/phenolic aldehyde-nitrile rubber after brushing adhesive stick and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) to subsides; Put into vulcanizing press or pressure-pot carries out hot pressing, hot pressing pressure is 2MPa, and hot pressing temperature is 80 DEG C, and the heat-insulation pressure keeping time is 30min, period, can decompression exhaust 3 times; After hot pressing terminates, be down to room temperature, take out prefabricated carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) subassembly (abbreviation prefabricated component);
4) cleanup step: motor body internal surface adopts technical grade ethyl acetate to clean out, and hangs 1h;
5) brush coating step: motor body inner homogeneous brushing adhesive stick, tackiness agent is CH205, and adhesive glue film thickness is 10 μm, hangs 2h; Then brush CH238, adhesive glue film thickness is 10 μm, hangs 2h;
6) placing step: prefabricated component is put into motor body preposition, the one side of the Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) of prefabricated component is fitted with motor body, available air or pressurize with Silicon rubber inflatable bag;
7) hot pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C, pressure 0.6MPa, heating, clamping time 1h, heat, pressurize complete, engine is taken out from heating unit;
8) flaw detection step: adopt digital ultrasonic flaw detector to Ethylene Propylene Terpolymer thermal insulation material (bottom) and the flaw detection of motor body adhesion interface, without occurring unsticking phenomenon, order is carried out;
9) curing schedule: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 160 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit;
10) cleaning step: clean with the carbon fiber/phenolic aldehyde-nitrile rubber of chemical pure ethyl acetate to the prefabricated component after solidification, by chemical pure ethyl acetate, Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is cleaned, hang 1h;
11) glue application step: the carbon fiber/phenolic aldehyde-nitrile rubber one side of prefabricated component after hardening brushes CH238, adhesive glue film thickness is 10 μm, hangs 2h, brushes CH238 at Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) simultaneously, adhesive glue film thickness is 10 μm, hangs 2h;
12) secondary placing step: Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is put into motor body preposition, Ethylene Propylene Terpolymer thermal insulation material (surface layer) and the carbon fiber/phenolic aldehyde-nitrile rubber be cured are fitted, available air or pressurize with Silicon rubber inflatable bag;
13) second heat pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C, pressure 0.6MPa, heating, clamping time 1h, heat, pressurize complete, engine is taken out from heating unit;
14) check step: Ethylene Propylene Terpolymer thermal insulation material (surface layer) surperficial bubble-free, order is carried out;
15) regelate step: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 160 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit.
This product is all crowned with complete success through ground experiment.Thermal insulation layer dissection and analysis after test, structural integrity between motor body/Ethylene Propylene Terpolymer thermal insulation material (bottom)/carbon fiber/phenolic aldehyde-nitrile rubber/Ethylene Propylene Terpolymer thermal insulation material (surface layer), without quality problems such as unsticking, gas enclosure pores, can meet design requirement completely.
Embodiment 3:
Certain solid propellant rocket, Ethylene Propylene Terpolymer thermal insulation material (bottom) 3mm is thick, and carbon fiber/phenolic aldehyde-nitrile rubber 2mm is thick, and Ethylene Propylene Terpolymer thermal insulation material (surface layer) 4mm is thick;
1) preliminary step: according to engine insulating structure dimensional requirement, by Ethylene Propylene Terpolymer thermal insulation material roller-compaction, by shaping for carbon fiber/phenolic aldehyde-nitrile rubber cutting;
2) squeegeeing step: adopt chemical pure ethyl acetate to clean out carbon fiber/phenolic aldehyde-nitrile rubber, hang 1h; Brushing CH238 glue, adhesive glue film gauge control, at 10 μm, hangs 2h; Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) adopts chemical pure ethyl acetate to clean out, and hangs 1h; Brushing CH238 glue, adhesive glue film gauge control, at 10 μm, hangs 2h;
3) prefabrication step: by the carbon fiber/phenolic aldehyde-nitrile rubber after brushing adhesive stick and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) to subsides; Put into vulcanizing press or pressure-pot carries out hot pressing, hot pressing pressure is 2MPa, and hot pressing temperature is 80 DEG C, and the heat-insulation pressure keeping time is 30min, period, can decompression exhaust 3 times; After hot pressing terminates, be down to room temperature, take out prefabricated carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) subassembly (abbreviation prefabricated component);
4) cleanup step: motor body internal surface adopts technical grade ethyl acetate to clean out, and hangs 1h;
5) brush coating step: motor body inner homogeneous brushing adhesive stick, tackiness agent is CH205, and adhesive glue film thickness is 10 μm, hangs 2h; Then brush CH238, adhesive glue film thickness is 10 μm, hangs 2h;
6) placing step: prefabricated component is put into motor body preposition, the one side of the Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) of prefabricated component is fitted with motor body, available air or pressurize with Silicon rubber inflatable bag;
7) hot pressing step: engine is inserted in heating unit, Heating temperature is 100 DEG C, pressure 0.6MPa, heating, clamping time 3h, heat, pressurize complete, engine is taken out from heating unit;
8) flaw detection step: adopt digital ultrasonic flaw detector to Ethylene Propylene Terpolymer thermal insulation material (bottom) and the flaw detection of motor body adhesion interface, without occurring unsticking phenomenon, order is carried out;
9) curing schedule: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 165 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit;
10) cleaning step: clean with the carbon fiber/phenolic aldehyde-nitrile rubber of chemical pure ethyl acetate to the prefabricated component after solidification, by chemical pure ethyl acetate, Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is cleaned, hang 1h;
11) glue application step: the carbon fiber/phenolic aldehyde-nitrile rubber one side of prefabricated component after hardening brushes CH238, adhesive glue film thickness is 10 μm, hangs 2h, brushes CH238 at Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) simultaneously, adhesive glue film thickness is 10 μm, hangs 2h;
12) secondary placing step: Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is put into motor body preposition, Ethylene Propylene Terpolymer thermal insulation material (surface layer) and the carbon fiber/phenolic aldehyde-nitrile rubber be cured are fitted, available air or pressurize with Silicon rubber inflatable bag;
13) second heat pressing step: engine is inserted in heating unit, Heating temperature is 100 DEG C, pressure 0.6MPa, heating, clamping time 2h, heat, pressurize complete, engine is taken out from heating unit;
14) check step: Ethylene Propylene Terpolymer thermal insulation material (surface layer) surperficial bubble-free, order is carried out;
15) regelate step: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 155 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit.
This product is all crowned with complete success through ground experiment.Thermal insulation layer dissection and analysis after test, structural integrity between motor body/Ethylene Propylene Terpolymer thermal insulation material (bottom)/carbon fiber/phenolic aldehyde-nitrile rubber/Ethylene Propylene Terpolymer thermal insulation material (surface layer), without quality problems such as unsticking, gas enclosure pores, can meet design requirement completely.
Embodiment 4:
Certain solid propellant rocket, Ethylene Propylene Terpolymer thermal insulation material (bottom) 3mm is thick, and carbon fiber/phenolic aldehyde-nitrile rubber 3mm is thick, and Ethylene Propylene Terpolymer thermal insulation material (surface layer) 2mm is thick;
1) preliminary step: according to engine insulating structure dimensional requirement, by Ethylene Propylene Terpolymer thermal insulation material roller-compaction, by shaping for carbon fiber/phenolic aldehyde-nitrile rubber cutting;
2) squeegeeing step: adopt chemical pure ethyl acetate to clean out carbon fiber/phenolic aldehyde-nitrile rubber, hang 1h; Brushing CH238 glue, adhesive glue film gauge control, at 5 μm, hangs 2h; Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) adopts chemical pure ethyl acetate to clean out, and hangs 1h; Brushing CH238 glue, adhesive glue film gauge control, at 5 μm, hangs 2h;
3) prefabrication step: by the carbon fiber/phenolic aldehyde-nitrile rubber after brushing adhesive stick and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) to subsides; Put into vulcanizing press or pressure-pot carries out hot pressing, hot pressing pressure is 2MPa, and hot pressing temperature is 80 DEG C, and the heat-insulation pressure keeping time is 30min, period, can decompression exhaust 2 times; After hot pressing terminates, be down to room temperature, take out prefabricated carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) subassembly (abbreviation prefabricated component);
4) cleanup step: motor body internal surface adopts technical grade ethyl acetate to clean out, and hangs 1h;
5) brush coating step: motor body inner homogeneous brushing adhesive stick, tackiness agent is CH205, and adhesive glue film thickness is 5 μm, hangs 2h; Then brush CH238, adhesive glue film thickness is 5 μm, hangs 2h;
6) placing step: prefabricated component is put into motor body preposition, the one side of the Ethylene Propylene Terpolymer thermal insulation of materials material (bottom) of prefabricated component is fitted with motor body, available air or pressurize with Silicon rubber inflatable bag;
7) hot pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C, pressure 1.0MPa, heating, clamping time 3h, heat, pressurize complete, engine is taken out from heating unit;
8) flaw detection step: adopt digital ultrasonic flaw detector to Ethylene Propylene Terpolymer thermal insulation material (bottom) and the flaw detection of motor body adhesion interface, without occurring unsticking phenomenon, order is carried out;
9) curing schedule: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 165 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit;
10) cleaning step: clean with the carbon fiber/phenolic aldehyde-nitrile rubber of chemical pure ethyl acetate to the prefabricated component after solidification, by chemical pure ethyl acetate, Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is cleaned, hang 1h;
11) glue application step: the carbon fiber/phenolic aldehyde-nitrile rubber one side of prefabricated component after hardening brushes CH238, adhesive glue film thickness is 5 μm, hangs 2h, brushes CH238 at Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) simultaneously, adhesive glue film thickness is 5 μm, hangs 2h;
12) secondary placing step: Ethylene Propylene Terpolymer thermal insulation of materials material (surface layer) is put into motor body preposition, Ethylene Propylene Terpolymer thermal insulation material (surface layer) and the carbon fiber/phenolic aldehyde-nitrile rubber be cured are fitted, available air or pressurize with Silicon rubber inflatable bag;
13) second heat pressing step: engine is inserted in heating unit, Heating temperature is 90 DEG C, pressure 0.8MPa, heating, clamping time 2h, heat, pressurize complete, engine is taken out from heating unit;
14) check step: Ethylene Propylene Terpolymer thermal insulation material (surface layer) surperficial bubble-free, order is carried out;
15) regelate step: inserted by engine in heating unit, after pressurization, is warming up to 105 DEG C, insulation 2h, and then temperature control rises to 160 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 95 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.0MPa; Engine is taken out from heating unit.
This product is all crowned with complete success through ground experiment.Thermal insulation layer dissection and analysis after test, structural integrity between motor body/Ethylene Propylene Terpolymer thermal insulation material (bottom)/carbon fiber/phenolic aldehyde-nitrile rubber/Ethylene Propylene Terpolymer thermal insulation material (surface layer), without quality problems such as unsticking, gas enclosure pores, can meet design requirement completely.

Claims (6)

1. the adhering method of carbon fiber/phenolic aldehyde-nitrile rubber, it is characterized in that, comprise motor body bonding successively, Ethylene Propylene Terpolymer thermal insulation of materials material, carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials material, its concrete bonding step is:
1) preliminary step: according to engine insulating structure dimensional requirement, by Ethylene Propylene Terpolymer thermal insulation material roller-compaction, by shaping for carbon fiber/phenolic aldehyde-nitrile rubber cutting; When there is end socket position, adopt mould compression molding;
2) squeegeeing step: carbon fiber/phenolic aldehyde-nitrile rubber is cleaned out, hangs 1 ~ 2h; Brushing CH238 tackiness agent, adhesive glue film gauge control, at 5 μm ~ 10 μm, hangs 1 ~ 2h or takes air blast or heating measures; Ethylene Propylene Terpolymer thermal insulation of materials material is cleaned out, and hangs 1 ~ 2h; Brushing CH238 glue, adhesive glue film gauge control, at 5 μm ~ 10 μm, hangs 1 ~ 2h or takes air blast or heating measures;
3) prefabrication step: by the carbon fiber/phenolic aldehyde-nitrile rubber after brushing adhesive stick and Ethylene Propylene Terpolymer thermal insulation of materials material to subsides; Put into vulcanizing press or pressure-pot carries out hot pressing, hot pressing pressure is 1MPa ~ 2MPa, and hot pressing temperature is 70 DEG C ~ 80 DEG C, and the heat-insulation pressure keeping time is 30min ~ 60min, period, decompression exhaust 2 ~ 3 times; After hot pressing terminates, be down to room temperature, take out prefabricated carbon fiber/phenolic aldehyde-nitrile rubber and Ethylene Propylene Terpolymer thermal insulation of materials combination of materials part;
4) cleanup step: motor body internal surface adopts the one in technical grade ethyl acetate, trichloromethane or acetone to clean out, and hangs 1 ~ 2h or takes air blast or heating measures;
5) brush coating step: motor body inner homogeneous brushing adhesive stick, tackiness agent is CH205, and adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h; Then brush CH238, adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h;
6) placing step: by 3) in the subassembly of gained put into motor body preposition, the one side of the Ethylene Propylene Terpolymer thermal insulation of materials material of subassembly is fitted with motor body, pressurizes with air or with Silicon rubber inflatable bag;
7) hot pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C ~ 100 DEG C, pressure 0.6MPa ~ 1.0MPa, heating, clamping time 1h ~ 3h, heat, pressurize complete, engine is taken out from heating unit;
8) flaw detection step: adopt digital ultrasonic flaw detector to Ethylene Propylene Terpolymer thermal insulation material and the flaw detection of motor body adhesion interface, check whether and occur unsticking phenomenon, be, go to step 8), otherwise order is carried out;
9) curing schedule: inserted by engine in heating unit, after pressurization, is warming up to 110 DEG C ± 5 DEG C, insulation 2h, and then temperature control rises to 165 DEG C ± 5 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 100 DEG C ± 5 DEG C again, and cooling rate is 15 DEG C/h, then is down to room temperature; Therebetween, pressure 1.1MPa ± 0.1MPa; Engine is taken out from heating unit;
10) cleaning step: the carbon fiber/phenolic aldehyde-nitrile rubber of the subassembly after solidification is cleaned, simultaneously to Ethylene Propylene Terpolymer material clean, hangs 1h ~ 2h or take air blast or heating measures;
11) glue application step: the carbon fiber/phenolic aldehyde-nitrile rubber one side of subassembly after hardening brushes CH238, and adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h;
12) secondary placing step: Ethylene Propylene Terpolymer thermal insulation of materials material is put into motor body preposition, Ethylene Propylene Terpolymer thermal insulation material and the carbon fiber/phenolic aldehyde-nitrile rubber be cured are fitted, and pressurize with air or with Silicon rubber inflatable bag;
13) second heat pressing step: engine is inserted in heating unit, Heating temperature is 80 DEG C ~ 100 DEG C, pressure 0.6MPa ~ 1.0MPa, heating, clamping time 1h ~ 3h, heat, pressurize complete, engine is taken out from heating unit;
14) step is checked: check whether Ethylene Propylene Terpolymer thermal insulation material surface occurs bubble, existence then adopts pinprick, tiltedly cuts mode degasification, then goes to step 13), otherwise carry out subsequent disposal;
15) regelate step: inserted by engine in heating unit, after being forced into 1.1MPa ± 0.1MPa, is warming up to 110 DEG C ± 5 DEG C, insulation 2h, and then temperature control rises to 165 DEG C ± 5 DEG C, and heat-up rate is 15 DEG C/h, insulation 1h; Temperature control is down to 100 DEG C ± 5 DEG C again, and cooling rate is 15 DEG C/h, is finally down to room temperature, takes out engine and namely completes the bonding process of carbon fiber/phenolic aldehyde-nitrile rubber as thermal insulation material.
2. method according to claim 1, is characterized in that: described 2) squeegeeing step and 10) in cleaning step, adopt chemical pure ethyl acetate to carry out clean.
3. method according to claim 1, is characterized in that: described 2) squeegeeing step, 4) cleanup step and 10) in cleaning step, blasting time is 1 ~ 2h.
4. method according to claim 1, is characterized in that: described 2) squeegeeing step, 4) cleanup step and 10) in cleaning step, the temperature of heating measures is 50 DEG C ~ 60 DEG C, and the time is 1 ~ 2h.
5. method according to claim 1, it is characterized in that: described 5) in brush coating step, while to motor body inner homogeneous brushing adhesive stick, brush CH238 in the Ethylene Propylene Terpolymer thermal insulation of materials material one side of subassembly, adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h.
6. method according to claim 1, is characterized in that: described 11) in glue application step, and simultaneously at Ethylene Propylene Terpolymer thermal insulation of materials material brushing CH238, adhesive glue film thickness is 5 μm ~ 10 μm, hangs 1h ~ 2h.
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CN107312482A (en) * 2017-07-28 2017-11-03 中国地质大学(武汉) Bullion makes the pouring procedure of epoxy resin AB glue
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CN107312482B (en) * 2017-07-28 2019-11-15 中国地质大学(武汉) The pouring procedure of epoxy resin AB glue in bullion production
CN107312482A (en) * 2017-07-28 2017-11-03 中国地质大学(武汉) Bullion makes the pouring procedure of epoxy resin AB glue
CN108839400A (en) * 2018-06-28 2018-11-20 湖北三江航天江北机械工程有限公司 Intermediate course formula is insulated layer material and preparation method thereof
CN109058661A (en) * 2018-07-27 2018-12-21 西安长峰机电研究所 A kind of interlayer composite adiabatic layer structure and manufacturing method
CN109605776A (en) * 2018-11-15 2019-04-12 湖北三江航天江北机械工程有限公司 Fiber wound and solidified rocket engine multiphase heat insulation layer forming method
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CN110256975A (en) * 2019-05-24 2019-09-20 上海航天化工应用研究所 A method of improving rubber and fabric adhesive strength
CN110256975B (en) * 2019-05-24 2021-07-13 上海航天化工应用研究所 Method for improving bonding strength of rubber and fiber fabric
CN111396216A (en) * 2020-03-18 2020-07-10 西安近代化学研究所 Basket type igniter of rotary solid rocket engine
CN114292596A (en) * 2021-12-08 2022-04-08 上海复合材料科技有限公司 Cementing method for inner heat insulation of ethylene propylene diene monomer in solid engine
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