CN101259766B - Polymer/porous ceramics structure and function integrated gradient composite material and preparation method thereof - Google Patents
Polymer/porous ceramics structure and function integrated gradient composite material and preparation method thereof Download PDFInfo
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- CN101259766B CN101259766B CN200810064327XA CN200810064327A CN101259766B CN 101259766 B CN101259766 B CN 101259766B CN 200810064327X A CN200810064327X A CN 200810064327XA CN 200810064327 A CN200810064327 A CN 200810064327A CN 101259766 B CN101259766 B CN 101259766B
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Abstract
The invention relates to a function-integration gradient composite material with polymer/porous ceramic structure and a preparation method. The invention solves the problems that single material can not meet the requirement for the performance of the material made by the application condition in an extreme environment and the multilayer composite-structure material is easily layered and has poor safety and reliability. The product of the invention is made from a polymer layer, a gradient connecting layer and a ceramic layer from the inside to the outside. The preparation method comprises the following steps that: 1. the polymer layer, the gradient connecting layer and the ceramic layer are sequentially paved and then are put into a die to be formed by compression so as to obtain the green body of the composite material; 2. the ceramic layer of the green body of the composite material is loaded with high-density heat flux and then is naturally cooled. The composite-structure material of the invention has the advantages of small weight, strong structural strength and high effective heat insulation, is suitable for being used under the extreme working conditions of high temperature, airflow washout, etc., and is safe as well as reliable. The preparation method of the invention is simple and easy to be operated, and can prepare large-scale products with a complicated shape.
Description
Technical field
The present invention relates to a kind of functional gradient composite materials and preparation method thereof.
Background technology
When aerospace craft (guided missile, rocket, airship etc.) is gone out atmosphere and returned ground with hypersonic speed (reentering), its surface temperature can reach 1000-5000 ℃ under pneumatic heating, will stand high pressure draught ablation and particle cloud in addition and corrode; During solid propellant rocket work, combustion chamber pressure can reach 20 atmospheric pressure, produces nearly 4000 ℃ high temperature, and combustion gas reaches the mach one number at the flow velocity at spray larynx place.Require aircraft energy follow-on mission under such environment, various devices and system's operate as normal must solve bullet solar heat protection and structure problem.
Metal and alloy were because their outstanding structural strengths and resistance to elevated temperatures once were used as the bullet material, but easy fusion distortion under the Yin Gaowen, and quality is overweight by the polymer matrix composite replacement of light weight relatively.Polymer such as phenolic resins, poly-aryl ethane, BMI, polyimides, epoxy resin have been widely studied and have used, the advantage that they generally have is light weight, mechanical strength height, but when guided missile during near high-speed flight, material surface energy reaches 1200 ℃ within short-term (less than 2 minutes), such temperature is far away on the temperature of depolymerization and destruction.Therefore, these traditional materials have been difficult to use separately and have satisfied the requirement to material of strategic missile that flying speed improves constantly.
At present, the spacecraft material develops to multi-level composite construction direction, and for example a kind of material that typically is designed to substantially is made of outer ablation layer, load-carrying construction layer, thermal insulation layer and aluminium honeycomb heat dissipating layer.But the shortcoming of this design is that it is the sandwich construction that is made of a variety of materials, and the performance difference between each layer is very big, makes that the security reliability of interface layer combination is poor.To cause the accident of the U.S. " Colombia " number space shuttle be exactly one of illustration because of part fritter heat barrier foam comes off.
Summary of the invention
The objective of the invention is to satisfy of the requirement of extreme environment service condition to material property in order to solve homogenous material, reach the problem of the easy layering of multi-layer compound structure material, security reliability difference, and polymer/porous ceramics structure and function integrated gradient composite material and preparation method thereof is provided.Product of the present invention has both the structural strength of polymeric matrix and porous ceramics is heat-resisting and the excellent properties of effectively insulating.Product of the present invention suits to use in extreme condition of work such as high temperature, airflow scouring, makes aerospace craft use material to realize that solar heat protection is simultaneously structure-integrated, improves the security reliability of using.
Polymer/porous ceramics structure and function integrated gradient composite material of the present invention is to be made by polymeric layer, gradient articulamentum and ceramic layer from the inside to the outside; Polymeric layer is to be made by polymer impregnated fibre reinforcement; The gradient articulamentum is to be made by the fibre reinforcement of polymer and ceramic size dipping, and wherein the gradient articulamentum has two to five layers, and from inside to outside the concentration gradients of the ceramic size of each layer increases and the polymer content gradient reduces in the gradient articulamentum; Ceramic layer is to be made by the fibre reinforcement of ceramic size dipping.Can also in the ceramic size of the ceramic layer of polymer/porous ceramics structure and function integrated gradient composite material, add hollow glass micropearl or the hollow SiO that all accounts for ceramic size cumulative volume 5%～30%
2Microballoon.
The preparation of present embodiment polymer/porous ceramics structure and function integrated gradient composite material realizes by following step: one, lay polymeric layer with polymer impregnated fibre reinforcement; The back impregnation of fibers that respectively polymer and ceramic size is mixed then strengthens body, on polymeric layer, lay two to five substratums again, obtain the gradient articulamentum, the concentration gradients of the ceramic size of each substratum increases and the polymer content gradient reduces in the gradient articulamentum from the inside to the outside; Fibre reinforcement with the ceramic size dipping is laid on the gradient articulamentum again, obtains ceramic layer; Put into the mould compression molding then: 150～340 ℃ of molding temperatures, molding pressure 1～10MPa, clamp time 2～10 hours, moulding finishes and obtains composite body; Two, that face of composite body ceramic layer is added the loading high-density hot-fluid, heat time heating time 3～60min, 500～1500 ℃ of ceramic layer surface temperatures, finish nature cooling of heating obtains polymer/porous ceramics structure and function integrated gradient composite material.Can also in the ceramic size of the ceramic layer of polymer/porous ceramics structure and function integrated gradient composite material, add hollow glass micropearl or the hollow SiO that all accounts for ceramic size cumulative volume 5%～30%
2Microballoon.Wherein in step 1, add hollow glass micropearl or the hollow SiO that all accounts for ceramic size cumulative volume 5%～30% in the ceramic size of ceramic layer
2Microballoon.
Fibre reinforcement in above-mentioned gradient articulamentum and the ceramic layer is quartz fibre or glass fibre.Fibre reinforcement in the polymeric layer is a kind of in carbon fiber, quartz fibre, glass fibre, Kevlar fiber, pbo fiber, the silicon carbide fibre.Ceramic size is made up of ceramic powder and organosilicon precursor, and described ceramic powder consumption accounts for 20%～70% of organosilicon precursor weight; Ceramic powder is SiC, TiC, WC, ZrC, Si
3N
4, TiN, AlN, BN, Al
2O
3, SiO
2, ZrO
2, Y
2O
3In one or more combination, the particle diameter of ceramic powder is between 20nm～20 μ m; The organosilicon precursor is organic polysilazane, organic poly-silicon-carbon alkane or organopolysiloxane.Polymer in polymeric layer and the gradient articulamentum is the organic resin that can solidify in 150 ℃～340 ℃ temperature ranges, specifically is BMI, polyimides, epoxy resin, phenolic resins or organic siliconresin.
Product of the present invention is close-connected integral body, do not have tangible boundary layer, and this structure has reduced the probability of the layering of material interface place, Xie Jian.The present invention adopts the mode of one-sided thermal source heating, makes the ceramic layer fast ceramicization, guarantees that two-layer (gradient articulamentum and polymeric layer) is affected little down.This function-graded material is on active service in extreme working environment still can keep excellent mechanical property, for material provides required structural strength.In addition, one-sided heating can make ceramic precursor along the cracking of temperature direction generation gradient, discharges micro-molecular gas, stays a large amount of pores in the cracking zone of transformation, forms gradient porous material.Porous material is referred to as " super insulating material "; because the gas conduction rate is generally than the low order of magnitude of solid nonmetallic materials thermal conductivity; being formed on when reducing density of material of loose structure; because the existence of gas in the porous material; reduced thermal conductivity by a relatively large margin, the interpolation of unlike material filler makes the heat transfer path of material complicated more; cause the material heat transfer property to descend significantly, thereby protected the electronic device of bottom polymer architecture and guided missile cone inside.When guided missile in high-speed flight, if be subjected to degrading of high-velocity particles cloud that the ceramic thermal barrier layer cavernous structure is caved in, the organosilicon presoma of lower floor can change porous ceramic structure rapidly under the hot-fluid effect, the performance heat insulating function is realized material self-shield effect.The present invention is prepared into porous ceramics with the top layer thermal insulation layer, be because porous ceramics combines that porous material density is little, light weight, specific area are big, than the good general characteristic of mechanics performance height, heat-proof quality and physics, the chemical stability of ceramic material, Heat stability is good, can not produce thermal deformation, softening, oxidative phenomena etc., operating temperature can be up to thousands of degrees centigrade.Polymer of the present invention/porous ceramics structure and function integrated gradient material has both the structural strength of polymeric matrix and porous ceramics is heat-resisting and the excellent properties of effectively insulating, can satisfy the requirement of the development of vehicle technology to material resistance to elevated temperatures and structural strength.
Sandwich of the present invention has the advantage of light weight, structural strength height and effectively insulating, suits to use under extreme condition of work such as high temperature, airflow scouring, and is safe and reliable.Easy, the easy operating of method of the present invention can prepare large complicated shape product.
Description of drawings
Fig. 1 is the schematic diagram that product of the present invention adopts one-sided heat source high temp heating; 1 expression thermal source among the figure, 2 expression ceramic layers, 3 expression gradient articulamentums, 4 expression polymeric layers.
The specific embodiment
The specific embodiment one: polymer/porous ceramics structure and function integrated gradient composite material is to be made by polymeric layer, gradient articulamentum and ceramic layer from the inside to the outside in the present embodiment; Polymeric layer is to be made by polymer impregnated fibre reinforcement; The gradient articulamentum is to be made by the fibre reinforcement of polymer and ceramic size dipping, and wherein the gradient articulamentum has two to five layers, and from inside to outside the concentration gradients of the ceramic size of each layer increases and the polymer content gradient reduces in the gradient articulamentum; Ceramic layer is to be made by the fibre reinforcement of ceramic size dipping.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the fibre reinforcement in the gradient articulamentum is quartz fibre or glass fibre.Other is identical with the specific embodiment one.
The form of present embodiment fibre reinforcement is chopped strand, continuous fiber or fibre three-dimensional fabric.
The specific embodiment three: what present embodiment and the specific embodiment one were different is: the fibre reinforcement in the ceramic layer is quartz fibre or glass fibre.Other is identical with the specific embodiment one.
The form of present embodiment fibre reinforcement is chopped strand, continuous fiber or fibre three-dimensional fabric.
The specific embodiment four: what present embodiment and the specific embodiment one were different is: the fibre reinforcement in the polymeric layer is a kind of in carbon fiber, quartz fibre, glass fibre, Kevlar fiber, pbo fiber, the silicon carbide fibre.Other is identical with the specific embodiment one.
But the form chopped strand of present embodiment fibre reinforcement, continuous fiber or fibre three-dimensional fabric.
The specific embodiment five: what present embodiment and the specific embodiment one were different is also to have added hollow glass micropearl or the hollow SiO that all accounts for ceramic size cumulative volume 5%～30% in the ceramic size of ceramic layer
2Microballoon.Other is identical with the specific embodiment one.
Add hollow glass micropearl or hollow SiO
2Microballoon can make composite comprise more pore structure, thereby the heat-proof quality of composite is further improved, architecture quality that simultaneously can lightening material.
The specific embodiment six: what present embodiment was different with the specific embodiment one or five is that ceramic size is made up of ceramic powder and organosilicon precursor, and described ceramic powder consumption accounts for 20%～70% of organosilicon precursor weight; Ceramic powder is SiC, TiC, WC, ZrC, Si
3N
4, TiN, AlN, BN, Al
2O
3, SiO
2, ZrO
2, Y
2O
3In one or more combination, the particle diameter of ceramic powder is between 20nm～20 μ m; The organosilicon precursor is organic polysilazane, organic poly-silicon-carbon alkane or organopolysiloxane.Other is identical with the specific embodiment one or five.
When the present embodiment ceramic powder is mixture, can be between various ceramic powders by any than mixing.
The specific embodiment seven: present embodiment and the specific embodiment six differences are that the organosilicon precursor is organic poly-silicon-carbon alkane or organic polysilazane.Other is identical with the specific embodiment six.
Adopt the organosilicon precursor of present embodiment, the porous ceramics skeleton structure that made by heat deflection is Si-C or Si-N, and when adopting present embodiment, the mechanical property that obtains product improves, but manufacturing cost is bigger.
The specific embodiment eight: present embodiment and the specific embodiment five are different is that the particle diameter of ceramic powder is 0.35～0.8 μ m.Other is identical with the specific embodiment five.
Adopted the ceramic powder of submicron order to can further improve the mechanical performance and the heat-proof quality of material in the present embodiment.
The specific embodiment nine: what present embodiment and the specific embodiment one were different is: the polymer in polymeric layer and the gradient articulamentum is the organic resin that can solidify in 150 ℃～340 ℃ temperature ranges, specifically is BMI, polyimides, epoxy resin, phenolic resins or organic siliconresin.Other is identical with the specific embodiment one.
The specific embodiment ten: the preparation of present embodiment polymer/porous ceramics structure and function integrated gradient composite material realizes by following step: one, lay polymeric layer with polymer impregnated fibre reinforcement; The back impregnation of fibers that respectively polymer and ceramic size is mixed then strengthens body, on polymeric layer, lay two to five substratums again, obtain the gradient articulamentum, the concentration gradients of the ceramic size of each layer increases and the polymer content gradient reduces in the gradient articulamentum from the inside to the outside; Fibre reinforcement with the ceramic size dipping is laid on the gradient articulamentum again, obtains ceramic layer; Put into the mould compression molding then: 150～340 ℃ of molding temperatures, molding pressure 1～10MPa, clamp time 2～10 hours, moulding finishes and obtains composite body; Two, that face of composite body ceramic layer is added the loading high-density hot-fluid, heat time heating time 3～60min, 500～1500 ℃ of ceramic layer surface temperatures, finish nature cooling of heating obtains polymer/porous ceramics structure and function integrated gradient composite material.
The gradient cracking takes place along the direction of heat flow pottery in step 2 in ceramic layer, discharge micro-molecular gas, forms the porous graded ceramics.
The specific embodiment 11: present embodiment and the specific embodiment ten are different is also to have added hollow glass micropearl or the hollow SiO that all accounts for ceramic size cumulative volume 5%～30% in the ceramic size of ceramic layer in step 1
2Microballoon.Other is identical with the specific embodiment ten.
Add hollow glass micropearl or hollow SiO
2Microballoon can make composite comprise more pore structure, thereby the heat-proof quality of composite is further improved, architecture quality that simultaneously can lightening material.
The specific embodiment 12: what present embodiment was different with the specific embodiment ten or 11 is that ceramic size is made up of ceramic powder and organosilicon precursor, and described ceramic powder consumption accounts for 20%～70% of organosilicon precursor weight; Ceramic powder is SiC, TiC, WC, ZrC, Si
3N
4, TiN, AlN, BN, Al
2O
3, SiO
2, ZrO
2, Y
2O
3In one or more combination, the particle diameter of ceramic powder is between 20nm～20 μ m; The organosilicon precursor is organic polysilazane, organic poly-silicon-carbon alkane or organopolysiloxane.Other is identical with the specific embodiment ten or 11.
When the present embodiment ceramic powder is mixture, can be between various ceramic powders by any than mixing.
The specific embodiment 13: present embodiment and the specific embodiment 12 differences are that the organosilicon precursor is organic poly-silicon-carbon alkane or organic polysilazane; Should carry out under the closed environment of starvation when in the step 2 that face of composite body ceramic layer being added the loading high-density hot-fluid, filling with inert gas in the confined chamber is as argon gas or helium.Other is identical with the specific embodiment 12.
Adopt the organosilicon precursor of present embodiment, the porous ceramics skeleton structure that made by heat deflection is Si-C or Si-N, and when adopting present embodiment, the mechanical property that obtains product improves, but manufacturing cost is bigger.
The specific embodiment 14: present embodiment and the specific embodiment 12 are different is that the particle diameter of ceramic powder is 0.35～0.8 μ m.Other is identical with the specific embodiment 12.
Adopted the ceramic powder of submicron order to can further improve the mechanical performance and the heat-proof quality of material in the present embodiment.
The specific embodiment 15: what present embodiment and the specific embodiment ten were different is: the polymer in the step 1 in polymeric layer and the gradient articulamentum is the organic resin that can solidify in 150 ℃～340 ℃ temperature ranges, specifically is BMI, polyimides, epoxy resin, phenolic resins or organic siliconresin.Other is identical with the specific embodiment ten.
The specific embodiment 16: the preparation of present embodiment polymer/porous ceramics structure and function integrated gradient composite material realizes by following step: one, lay two to 15 layers with polymer impregnated fibre reinforcement, obtain polymeric layer; Respectively polymer and ceramic size are strengthened body by the quality gradual change back impregnation of fibers that is mixed then, on polymeric layer, lay four layers again, obtain the gradient articulamentum, from the inside to the outside, be fibre reinforcement successively by 80wt% polymer and 20wt% ceramic size dipping, the fibre reinforcement of 40wt% polymer and 60wt% ceramic size dipping, the fibre reinforcement of 60wt% polymer and 40wt% ceramic size dipping, the fibre reinforcement of 20wt% polymer and 40wt% ceramic size dipping is laid and is formed; On the gradient articulamentum, lay two to 15 layers again, obtain ceramic layer with the fibre reinforcement of ceramic size dipping; Put into the mould compression molding then: 150～340 ℃ of molding temperatures, molding pressure 1～10MPa, clamp time 2～10 hours, moulding finishes and obtains composite body; Two, that face of composite body ceramic layer is added the loading high-density hot-fluid, heat time heating time 3～60min, 500～1500 ℃ of ceramic layer surface temperatures, finish nature cooling of heating obtains polymer/porous ceramics structure and function integrated gradient composite material.
The specific embodiment 17: what present embodiment and the specific embodiment 16 were different is: polymeric layer is to be made by the carbon fiber of bimaleimide resin dipping in the step 1; The organosilicon precursor of ceramic layer is a polymethyl siloxane, has added the SiO of average grain diameter at 1 μ m in the ceramic size
2Superfine powder, polymethyl siloxane and SiO
2The ratio of ceramic powder mass fraction is 4: 1, and the fibre reinforcement of gradient articulamentum and ceramic layer is a quartz fibre; 180 ℃～220 ℃ of molding temperatures, clamp time 6 hours, molding pressure 3～5MPa.Other is identical with the specific embodiment 16.
The specific embodiment 18: present embodiment and the specific embodiment 17 differences are to prepare the polymethyl siloxane and the SiO of ceramic layer raw material
2The ratio of the mass fraction of ceramic powder is 1: 1, can below 120 ℃ polymethyl siloxane heated 5～60 minutes in advance before the dipping.Other is with specifically enforcement 17 is identical.When adopting present embodiment, the viscosity of ceramic size raises, and to improve the dipping ability of ceramic size to fiber, volume contraction is little in the material cracking process of present embodiment preparation with the preheating of organosilicon precursor elder generation.
Claims (9)
1. polymer/porous ceramics structure and function integrated gradient composite material is characterized in that polymer/porous ceramics structure and function integrated gradient composite material is to be made by polymeric layer, gradient articulamentum and ceramic layer from the inside to the outside; Polymeric layer is to be made by polymer impregnated fibre reinforcement; The gradient articulamentum is to be made by the fibre reinforcement of polymer and ceramic size dipping, and wherein the gradient articulamentum is divided into two to five substratums, and from inside to outside the concentration gradients of each substratum ceramic size increases and the polymer content gradient reduces in the gradient articulamentum; Ceramic layer is to be made by the fibre reinforcement of ceramic size dipping; The hollow glass micropearl or the hollow SiO that account for ceramic size cumulative volume 5%～30% in the ceramic size of ceramic layer, have also been added
2Microballoon.
2. polymer/porous ceramics structure and function integrated gradient composite material according to claim 1 is characterized in that the fibre reinforcement in gradient articulamentum and the ceramic layer is quartz fibre or glass fibre.
3. polymer/porous ceramics structure and function integrated gradient composite material according to claim 1 is characterized in that fibre reinforcement in the polymeric layer is a kind of in carbon fiber, quartz fibre, glass fibre, Kevlar fiber, pbo fiber, the silicon carbide fibre.
4. polymer/porous ceramics structure and function integrated gradient composite material according to claim 1, it is characterized in that ceramic size is made up of ceramic powder and organosilicon precursor, described ceramic powder consumption accounts for 20%～70% of organosilicon precursor weight.
5. polymer/porous ceramics structure and function integrated gradient composite material according to claim 4 is characterized in that ceramic powder is SiC, TiC, WC, ZrC, Si
3N
4, TiN, AlN, BN, Al
2O
3, SiO
2, ZrO
2, Y
2O
3In one or more combination, the particle diameter of ceramic powder is between 20nm～20 μ m.
6. polymer/porous ceramics structure and function integrated gradient composite material according to claim 5, the particle diameter that it is characterized in that ceramic powder are 0.35～0.8 μ m.
7. polymer/porous ceramics structure and function integrated gradient composite material according to claim 4 is characterized in that the organosilicon precursor is organic polysilazane, organic poly-silicon-carbon alkane or organopolysiloxane.
8. polymer/porous ceramics structure and function integrated gradient composite material according to claim 1 is characterized in that the polymer in polymeric layer and the gradient articulamentum is BMI, polyimides, epoxy resin, phenolic resins or organic siliconresin.
9. the method for preparing the described polymer/porous ceramics structure and function integrated gradient composite material of claim 1 is characterized in that the preparation of polymer/porous ceramics structure and function integrated gradient composite material realizes by following step: one, lay polymeric layer with polymer impregnated fibre reinforcement; The back impregnation of fibers that respectively polymer and ceramic size is mixed then strengthens body, on polymeric layer, lay two to five substratums again, obtain the gradient articulamentum, the concentration gradients of the ceramic size of each substratum increases and the polymer content gradient reduces in the gradient articulamentum from the inside to the outside; Fibre reinforcement with the ceramic size dipping is laid on the gradient articulamentum again, obtains ceramic layer; Put into the mould compression molding then: 150～340 ℃ of molding temperatures, molding pressure 1～10MPa, clamp time 2～10 hours, moulding finishes and obtains composite body; Two, composite body pottery aspect is loaded the high density hot-fluid, heat time heating time 3～60min, 500～1500 ℃ of ceramic layer surface temperatures, the heating nature cooling that finishes obtains polymer/porous ceramics structure and function integrated gradient composite material; Wherein in step 1, add hollow glass micropearl or the hollow SiO that all accounts for ceramic size cumulative volume 5%～30% in the ceramic size of ceramic layer
2Microballoon.
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| 宋仁义.先驱体转化法制备无机基/有机聚合物梯度材料.中国优秀博硕士学位论文全文数据库（博士）工程科技Ⅰ辑 2006年第12期.2006,(2006年第12期),B020-10，第10-12、89-90页. |
| 宋仁义.先驱体转化法制备无机基/有机聚合物梯度材料.中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑 2006年第12期.2006,(2006年第12期),B020-10,全文. * |
| 宋仁义.先驱体转化法制备无机基/有机聚合物梯度材料.中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑 2006年第12期.2006,(2006年第12期),B020-10,第10-12、89-90页. * |
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