CN103936390B - The preparation method of phosphate composite material antenna house cover body - Google Patents
The preparation method of phosphate composite material antenna house cover body Download PDFInfo
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- CN103936390B CN103936390B CN201410060342.2A CN201410060342A CN103936390B CN 103936390 B CN103936390 B CN 103936390B CN 201410060342 A CN201410060342 A CN 201410060342A CN 103936390 B CN103936390 B CN 103936390B
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Abstract
nullThe invention discloses the preparation method of a kind of phosphate composite material antenna house cover body，The method uses fiber cloth preimpregnation phosphate glue，Then laying、The molding of cure under pressure，It is prepared for phosphate composite material antenna house cover body，The firming agent of the present invention uses the multicomponent firming agent based on aluminium oxide，Not only improve curing rate and efficiency，And chromium oxide and zirconium oxide are heat-resisting up to 1700 DEG C，Thus further increase the resistance to elevated temperatures of composite，The technique that the present invention uses cure under pressure，Avoiding steam explosive vaporization in solidification process causes material structure loose and substantial amounts of voidage，Compactness and the mechanical property of in solidification process material have been effectively ensured，Simultaneously，The condition of cure that substep slowly heats up is also beneficial to gas and can discharge in time，Reduce the porosity of material internal，Be conducive to the compactness of material.The inventive method is simple, with short production cycle, and cost is relatively low, is suitable for through engineering approaches and produces.
Description
Technical field
The present invention relates to guided missile wave transparent antenna house preparing technical field, in particular to the preparation method of a kind of phosphate composite material antenna house cover body, can be applicable to air-ground, absolutely empty, the ship-based missile of short distance, intermediate range.
Background technology
Antenna house is positioned at the head of guided missile, is important feature parts of body, plays a part carrying, heat insulation, wave transparent, covers in severe flight environment of vehicle can normally work with radar antenna in protective cover.
Development along with aeronautical and space technology, the flight Mach number of missile weapon system improves constantly, and missile antenna cover material is had higher requirement by severe flight environment of vehicle, must bear higher temperature and thermal shock, meet excellent electrical property, at high temperature can keep higher mechanical strength etc..Traditional polymer matrix composites resistance to elevated temperatures is poor, Applicable temperature relatively low (the highest at 500 DEG C), is mainly used in low Mach, is difficult to meet the use requirement of high Mach missile-borne radome.Although studying and apply more quartzy composite ceramics, aluminium oxide ceramics, silicon nitride ceramics etc. to have electric property and the resistance to elevated temperatures of excellence at present, but ceramic material fragility is big, and damage tolerance is low, yield rate is low, and complex forming technology, relatively costly, limit it and be widely applied.
Summary of the invention
It is an object of the invention to the defect overcoming existing antenna house non-refractory, fragility is big, yield rate is low, complex process, cost are high, the preparation method of a kind of phosphate composite material antenna house cover body is provided, the method has the features such as with short production cycle, low cost, the antenna house cover body produced uses temperature range to be 600～1000 DEG C, it is possible to meet that brachymedial journey is air-ground, absolutely empty, the use requirement of ship-based missile.
For achieving the above object, the preparation method of the phosphate composite material antenna house cover body designed by the present invention, comprise the following steps:
1) the molding core of antenna cover body and outer mold are prepared, and pretreatment high silica fiber cloth or the fiber cloth of quartz fiber cloth gained, and according to antenna house cover body size and prescription, determine size and the laying quantity of fiber cloth；
2) uniform application releasing agent on molding core and outer mold；
3) with scraper phosphate glue it is coated onto in each piece of fiber cloth equably and rolls flat, then by the fiber cloth the most successively laying that coats on molding core, process of deployment often spreading two-layer, rolls once, it is ensured that fiber cloth surfacing；
4) after fiber cloth is laid, outer mold is sleeved on molding core, tightens the pressurization bolt of mould, apply pressure so that the fiber cloth between molding core and outer mold is compacted；
5) being then positioned in baking oven by cover body mould, be heating and curing, after having solidified, be cooled to room temperature, cover body blank is taken out in the demoulding；
6) to cover body blank machining to required size, phosphate composite material antenna house cover body is i.e. obtained.
Wherein, step 1) preprocess method of described high silica fiber cloth or quartz fiber cloth is: high silica fiber cloth or quartz fiber cloth are aoxidized to remove completely in the air of 200～300 DEG C the oxygen-containing polymers on its surface；The time of general oxidation is 1～3h, and oxygen-containing polymers is epoxy resin, poly-phthalimide, ethers etc.；Fiber cloth is in process of production, for avoiding winding, damage starching to be carried out process during weaving process, what surface was starched is mainly composed of oxygen-containing polymers, such as epoxy resin, poly-phthalimide, ethers etc., the presence of which can have a strong impact on the bond strength between fiber cloth and phosphate base body interface, therefore needing to carry out fiber cloth in the air of 200～300 DEG C oxidation processes, the time of oxidation is 1～3h, to remove the oxygen-containing polymers on its surface；
Step 3) compound method of described phosphate glue is: phosphate resin prepared according to the quality proportioning of 1:0.5～1 with firming agent, ground and mixed fully, obtain the glue of homogeneous (without solid particle existence, loop-like epoxy resins state), its viscosity is 1.0～1.25Pa S, then by glue standing 2～4h, standby.The viscosity of glue is that 1.0～1.25Pa S are more suitable, and viscosity is too small, and the mobility of glue is preferable, and the glue being attached in fiber cloth very little, can cause the phosphate matrix between scrim cloth to reduce, affect the performance of material；Viscosity is excessive, and the mobility of glue is poor, is deteriorated the effect of impregnation of fiber cloth, can cause the phosphate matrix skewness between scrim cloth, affect the stability of material property.
Preferably, described step 3) in, phosphate resin is aluminum phosphate resin or chrome-alumina phosphate resin.
Alternatively, described step 3) in, firming agent is the mixture of one or more in aluminium oxide, zirconium oxide, chromium oxide, and the granularity of described firming agent is micron order and nanoscale.
Preferably, described fiber cloth is pretreatment high silica fiber cloth or the fiber cloth of quartz fiber cloth gained, described step 3) in, firming agent is the mixture that weight ratio is 4～5:1 of aluminium oxide and chromium oxide.
Preferably, described step 3) in, firming agent be aluminium oxide, chromium oxide, zirconic weight ratio be the mixture of 7～8:1:2.
Preferably, described step 3) in, in fiber cloth consumption is fiber cloth weight 2～3 times of be coated with phosphate glue.
Preferably, described step 4) in, executing stressed size is 2～5MPa.
Preferably, described step 5) in, the condition being heating and curing is: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, is incubated 2～4h, is then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 2～4h, Temperature fall.
Beneficial effects of the present invention: using fiber cloth preimpregnation phosphate glue, then laying, the moulding technique of cure under pressure are prepared for phosphate composite material antenna house cover body, and advantage is as follows:
1) this process is simple, with short production cycle, and cost is relatively low, is suitable for through engineering approaches and produces.
2) firming agent of the present invention uses the multicomponent firming agent based on aluminium oxide, not only improves curing rate and efficiency, and chromium oxide and zirconium oxide are heat-resisting up to 1700 DEG C, thus further increase the resistance to elevated temperatures of composite.
3) present invention uses the process of cure under pressure, it is to avoid in solidification process, steam explosive vaporization causes material structure loose and substantial amounts of voidage, and compactness and the mechanical property of in solidification process material be effectively ensured.Meanwhile, the condition of cure that substep slowly heats up is also beneficial to gas and can discharge in time, reduces the porosity of material internal, the beneficially compactness of material.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The preparation of certain engineering short-range guided missile antenna house cover body:
1) prepare molding core and the outer mold of antenna cover body, according to antenna house cover body size and prescription, determine size and the laying quantity of high silica fiber cloth.
2) pretreatment of high silica fiber cloth: by it at 200 DEG C of air oxidation 2h, removes fiber cloth surface epoxy type polymer.
3) preparation of phosphate glue: chromium phosphate resin and firming agent (aluminium oxide: chromium oxide=4:1) are prepared according to the quality proportioning of 1:0.8, sufficient ground and mixed in a reservoir, until glue exists without solid particle, and in loop-like epoxy resins state, viscosity requirement is at 1.0～1.25Pa S.Then glue is stood 2h.
4) uniform application releasing agent on molding core and outer mold.
5) laying of prepreg cloth: the chromium phosphate glue of preparation is coated onto on pretreated high silica fiber cloth with scraper and rolls flat (chromium phosphate glue is 7:3 with the mass ratio of high silica fiber cloth) equably, then the high silica fiber cloth coated is layered on cover body molding core, it is desirable to fiber cloth is smooth, corrugationless.The most successively laying, often spreads two-layer, rolls once, it is ensured that fiber cloth surfacing, corrugationless.
6) laying is to the thickness set, and is sleeved on by outer mold on molding core, tightens the pressurization bolt of mould, applies the pressure of 2MPa.
7) then cover body mould is positioned in baking oven, solidifies according to following condition of cure: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, be incubated 2h, be then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 3h, Temperature fall.After having solidified, being cooled to room temperature, cover body blank is taken out in the demoulding.
8) to cover body blank machining to required size, i.e. can get phosphate composite material antenna house cover body.
Use the phosphate composite material antenna house cover body prepared of the present invention to stand actual working environment examination and without destroying: stationary point spot temperature 600～900 DEG C, large area temperature 400～500 DEG C.Product is as follows with stove sample performance:
| Bending strength (MPa) | Hot strength (MPa) | Dielectric constant | Dielectric loss angle tangent |
| 98 | 64 | 3.4 | 0.011 |
Embodiment 2
The preparation of certain engineering short-range guided missile antenna house cover body:
1) prepare molding core and the outer mold of antenna cover body, according to antenna house cover body size and prescription, determine size and the laying quantity of high silica fiber cloth.
2) pretreatment of high silica fiber cloth: by it at 200 DEG C of air oxidation 2h, removes fiber cloth surface epoxy type polymer.
3) preparation of phosphate glue: chromium phosphate resin and firming agent (aluminium oxide: chromium oxide=5:1) are prepared according to the quality proportioning of 1:0.8, sufficient ground and mixed in a reservoir, until glue exists without solid particle, and in loop-like epoxy resins state, viscosity requirement is at 1.0～1.25Pa S.Then glue is stood 2h.
4) uniform application releasing agent on molding core and outer mold.
5) laying of prepreg cloth: the chromium phosphate glue of preparation is coated onto on pretreated high silica fiber cloth with scraper and rolls flat (chromium phosphate glue is 7:3 with the mass ratio of high silica fiber cloth) equably, then the high silica fiber cloth coated is layered on cover body molding core, it is desirable to fiber cloth is smooth, corrugationless.The most successively laying, often spreads two-layer, rolls once, it is ensured that fiber cloth surfacing, corrugationless.
6) laying is to the thickness set, and is sleeved on by outer mold on molding core, tightens the pressurization bolt of mould, applies the pressure of 2MPa.
7) then cover body mould is positioned in baking oven, solidifies according to following condition of cure: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, be incubated 2h, be then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 3h, Temperature fall.After having solidified, being cooled to room temperature, cover body blank is taken out in the demoulding.
8) to cover body blank machining to required size, i.e. can get phosphate composite material antenna house cover body.
Use the phosphate composite material antenna house cover body prepared of the present invention to stand actual working environment examination and without destroying: stationary point spot temperature 600～900 DEG C, large area temperature 400～500 DEG C.Product is as follows with stove sample performance:
| Bending strength (MPa) | Hot strength (MPa) | Dielectric constant | Dielectric loss angle tangent |
| 95 | 65 | 3.38 | 0.011 |
Embodiment 3
The preparation of certain engineering short-range guided missile antenna house cover body:
1) prepare molding core and the outer mold of antenna cover body, according to antenna house cover body size and prescription, determine size and the laying quantity of high silica fiber cloth.
2) pretreatment of high silica fiber cloth: by it at 200 DEG C of air oxidation 2h, removes fiber cloth surface epoxy type polymer.
3) preparation of phosphate glue: chromium phosphate resin is prepared according to the quality proportioning of 1:0.8 with firming agent (aluminium oxide), sufficient ground and mixed in a reservoir, until glue exists without solid particle, and in loop-like epoxy resins state, viscosity requirement is at 1.0～1.25Pa S.Then glue is stood 2h.
4) uniform application releasing agent on molding core and outer mold.
5) laying of prepreg cloth: the chromium phosphate glue of preparation is coated onto on pretreated high silica fiber cloth with scraper and rolls flat (chromium phosphate glue is 7:3 with the mass ratio of high silica fiber cloth) equably, then the high silica fiber cloth coated is layered on cover body molding core, it is desirable to fiber cloth is smooth, corrugationless.The most successively laying, often spreads two-layer, rolls once, it is ensured that fiber cloth surfacing, corrugationless.
6) laying is to the thickness set, and is sleeved on by outer mold on molding core, tightens the pressurization bolt of mould, applies the pressure of 2MPa.
7) then cover body mould is positioned in baking oven, solidifies according to following condition of cure: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, be incubated 2h, be then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 3h, Temperature fall.After having solidified, being cooled to room temperature, cover body blank is taken out in the demoulding.
8) to cover body blank machining to required size, i.e. can get phosphate composite material antenna house cover body.
Use the phosphate composite material antenna house cover body prepared of the present invention to stand actual working environment examination and without destroying: stationary point spot temperature 600～900 DEG C, large area temperature 400～500 DEG C.Product is as follows with stove sample performance:
| Bending strength (MPa) | Hot strength (MPa) | Dielectric constant | Dielectric loss angle tangent |
| 90 | 59 | 3.4 | 0.011 |
Embodiment 4
The preparation of certain engineering intermediate range missile antenna house cover body:
1) prepare molding core and the outer mold of antenna cover body, according to antenna house cover body size and prescription, determine size and the laying quantity of quartz fiber cloth.
2) pretreatment of quartz fiber cloth: by it at 200 DEG C of air oxidation 2h, removes fiber cloth surface epoxy type polymer.
3) preparation of phosphate glue: chrome-alumina phosphate resin and firming agent (aluminium oxide: chromium oxide: zirconium oxide=7:1:2) are prepared according to the quality proportioning of 1:1, sufficient ground and mixed in a reservoir, until glue exists without solid particle, and becoming loop-like epoxy resins state, viscosity requirement is at 1.0～1.25Pa S.Then glue is stood 2h.
4) uniform application releasing agent on molding core and outer mold.
5) laying of prepreg cloth: the chrome-alumina phosphate glue of preparation is coated onto equably in pretreated quartz fiber cloth and rolls flat (chrome-alumina phosphate glue is 7:3 with the mass ratio of quartz fiber cloth) with scraper, then the quartz fiber cloth coated is layered on cover body molding core, it is desirable to fiber cloth is smooth, corrugationless.The most successively laying, often spreads two-layer, rolls once, it is ensured that fiber cloth surfacing, corrugationless.
6) laying is to the thickness set, and is sleeved on by outer mold on molding core, tightens the pressurization bolt of mould, applies the pressure of 2MPa.
7) then cover body mould is positioned in baking oven, solidifies according to following condition of cure: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, be incubated 3h, be then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 4h, Temperature fall.After having solidified, being cooled to room temperature, cover body blank is taken out in the demoulding.
8) to cover body blank machining to required size, i.e. can get phosphate composite material antenna house cover body.
Use the phosphate composite material antenna house cover body prepared of the present invention to stand actual working environment examination and without destroying: stationary point spot temperature 1000～1200 DEG C, large area temperature 600～800 DEG C.Product is as follows with stove sample performance:
| Bending strength (MPa) | Hot strength (MPa) | Dielectric constant | Dielectric loss angle tangent |
| 126 | 79 | 3.2 | 0.012 |
Embodiment 5
The preparation of certain engineering intermediate range missile antenna house cover body:
1) prepare molding core and the outer mold of antenna cover body, according to antenna house cover body size and prescription, determine size and the laying quantity of quartz fiber cloth.
2) pretreatment of quartz fiber cloth: by it at 200 DEG C of air oxidation 2h, removes fiber cloth surface epoxy type polymer.
3) preparation of phosphate glue: chrome-alumina phosphate resin and firming agent (aluminium oxide: chromium oxide: zirconium oxide=8:1:2) are prepared according to the quality proportioning of 1:1, sufficient ground and mixed in a reservoir, until glue exists without solid particle, and becoming loop-like epoxy resins state, viscosity requirement is at 1.0～1.25Pa S.Then glue is stood 2h.
4) uniform application releasing agent on molding core and outer mold.
5) laying of prepreg cloth: the chrome-alumina phosphate glue of preparation is coated onto equably in pretreated quartz fiber cloth and rolls flat (chrome-alumina phosphate glue is 7:3 with the mass ratio of quartz fiber cloth) with scraper, then the quartz fiber cloth coated is layered on cover body molding core, it is desirable to fiber cloth is smooth, corrugationless.The most successively laying, often spreads two-layer, rolls once, it is ensured that fiber cloth surfacing, corrugationless.
6) laying is to the thickness set, and is sleeved on by outer mold on molding core, tightens the pressurization bolt of mould, applies the pressure of 2MPa.
7) then cover body mould is positioned in baking oven, solidifies according to following condition of cure: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, be incubated 3h, be then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 4h, Temperature fall.After having solidified, being cooled to room temperature, cover body blank is taken out in the demoulding.
8) to cover body blank machining to required size, i.e. can get phosphate composite material antenna house cover body.
Use the phosphate composite material antenna house cover body prepared of the present invention to stand actual working environment examination and without destroying: stationary point spot temperature 1000～1200 DEG C, large area temperature 600～800 DEG C.Product is as follows with stove sample performance:
| Bending strength (MPa) | Hot strength (MPa) | Dielectric constant | Dielectric loss angle tangent |
| 120 | 82 | 3.2 | 0.012 |
Embodiment 6
The preparation of certain engineering intermediate range missile antenna house cover body:
1) prepare molding core and the outer mold of antenna cover body, according to antenna house cover body size and prescription, determine size and the laying quantity of quartz fiber cloth.
2) pretreatment of quartz fiber cloth: by it at 200 DEG C of air oxidation 2h, removes fiber cloth surface epoxy type polymer.
3) preparation of phosphate glue: chrome-alumina phosphate resin is prepared according to the quality proportioning of 1:1 with firming agent (aluminium oxide), sufficient ground and mixed in a reservoir, until glue exists without solid particle, and becoming loop-like epoxy resins state, viscosity requirement is at 1.0～1.25Pa S.Then glue is stood 2h.
4) uniform application releasing agent on molding core and outer mold.
5) laying of prepreg cloth: the chrome-alumina phosphate glue of preparation is coated onto equably in pretreated quartz fiber cloth and rolls flat (chrome-alumina phosphate glue is 7:3 with the mass ratio of quartz fiber cloth) with scraper, then the quartz fiber cloth coated is layered on cover body molding core, it is desirable to fiber cloth is smooth, corrugationless.The most successively laying, often spreads two-layer, rolls once, it is ensured that fiber cloth surfacing, corrugationless.
6) laying is to the thickness set, and is sleeved on by outer mold on molding core, tightens the pressurization bolt of mould, applies the pressure of 2MPa.
7) then cover body mould is positioned in baking oven, solidifies according to following condition of cure: with the heating rate of 10 DEG C/h by room temperature to 150 DEG C, be incubated 3h, be then warming up to 180 DEG C with the heating rate of 25 DEG C/h, be incubated 4h, Temperature fall.After having solidified, being cooled to room temperature, cover body blank is taken out in the demoulding.
8) to cover body blank machining to required size, i.e. can get phosphate composite material antenna house cover body.
Use the phosphate composite material antenna house cover body prepared of the present invention to stand actual working environment examination and without destroying: stationary point spot temperature 1000～1200 DEG C, large area temperature 600～800 DEG C.Product is as follows with stove sample performance:
| Bending strength (MPa) | Hot strength (MPa) | Dielectric constant | Dielectric loss angle tangent |
| 115 | 76 | 3.1 | 0.012 |
Claims (3)
1. a preparation method for phosphate composite material antenna house cover body, including following step
Rapid:
1) molding core and the outer mold of antenna cover body, and pretreatment high silica fiber are prepared
Cloth or the fiber cloth of quartz fiber cloth gained, and want according to antenna house cover body size and quality
Ask, determine size and the laying quantity of fiber cloth；
2) uniform application releasing agent on molding core and outer mold；
3) with scraper phosphate glue it is coated onto in each piece of fiber cloth equably and rolls flat,
Then by the fiber cloth the most successively laying that coats on molding core, every in process of deployment
Paving two-layer, rolls once, it is ensured that fiber cloth surfacing；
4), after fiber cloth is laid, outer mold is sleeved on molding core, tightens mould
The pressurization bolt of tool, applies pressure so that fiber cloth pressure between molding core and outer mold
Real；
5) being then positioned in baking oven by cover body mould, be heating and curing, solidification completes
After, it being cooled to room temperature, cover body blank is taken out in the demoulding；
6) to cover body blank machining to required size, phosphate composite material is i.e. obtained
Antenna house cover body；
Wherein, step 1) described high silica fiber cloth or the preprocess method of quartz fiber cloth
For: high silica fiber cloth or quartz fiber cloth are aoxidized with complete in the air of 200～300 DEG C
The full oxygen-containing polymers removing its surface；
Step 3) in, the compound method of described phosphate glue is: by phosphate resin with
Firming agent is prepared according to the quality proportioning of 1:0.5～1, ground and mixed fully,
To homogeneous glue, its viscosity is 1.0～1.25Pa S, then glue is stood 2～4h,
Standby；
Described phosphate resin is aluminum phosphate resin or chrome-alumina phosphate resin；
Described firming agent be aluminium oxide, chromium oxide and zirconic weight ratio be 7～8:1:2
Mixture；
Described step 5) in, the condition being heating and curing is: with the heating rate of 10 DEG C/h by
Room temperature, to 150 DEG C, is incubated 2～4h, is then warming up to the heating rate of 25 DEG C/h
180 DEG C, it is incubated 2～4h, Temperature fall.
The preparation of phosphate composite material antenna house cover body the most according to claim 1
Method, it is characterised in that: described step 3) in, be coated with phosphate glue in fiber cloth
Consumption is 2～3 times of fiber cloth weight.
The preparation of phosphate composite material antenna house cover body the most according to claim 1
Method, it is characterised in that: described step 4) in, executing stressed size is 2～5MPa.
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Cited By (1)
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| CN106626195A (en) * | 2016-12-23 | 2017-05-10 | 湖北三江航天江北机械工程有限公司 | Machining method for outer cover one-mold multi-cavity molding of antenna cover and molding device thereof |
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| CN106242550A (en) * | 2016-07-22 | 2016-12-21 | 哈尔滨工业大学 | A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof |
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