CN110451942A - A kind of growth in situ alumina whisker enhancing vitreous silica radome/antenna windows preparation method and application - Google Patents
A kind of growth in situ alumina whisker enhancing vitreous silica radome/antenna windows preparation method and application Download PDFInfo
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- CN110451942A CN110451942A CN201910827506.2A CN201910827506A CN110451942A CN 110451942 A CN110451942 A CN 110451942A CN 201910827506 A CN201910827506 A CN 201910827506A CN 110451942 A CN110451942 A CN 110451942A
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- radome
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q1/00—Details of, or arrangements associated with, antennas
- H01Q1/42—Housings not intimately mechanically associated with radiating elements, e.g. radome
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5276—Whiskers, spindles, needles or pins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The present invention provides a kind of growth in situ alumina whiskers to enhance vitreous silica radome/antenna windows preparation method, is to prepare the Al with specific molecular structure guiding by the way that using aluminum sulfate as raw material, hexamethylene diamine is model agent2O3Powder.Yttrium oxide powder is introduced as sintering aid, at high temperature in-situ preparation Al2O3Whisker.Al2O3Whisker large specific surface area, itself has high mechanical property.It as reinforcing material, can effectively increase the contact area with vitreous silica, improve the interfacial combined function of reinforcement and ceramic matrix.Under high-temperature work environment, Al2O3Whisker performance is stablized, and plays the role of bridging matrix micro-cracks, improves radome/antenna windows high-temperature behavior and thermal shock resistance.
Description
Technical field
The invention belongs to high temperature manufacturing technology field, in particular to a kind of growth in situ alumina whisker enhances vitreous silica
Radome/antenna windows preparation method and application.
Background technique
Radome/antenna windows are to be located at Vehicle nose, the important equipment that protection radar system works normally.Melting
Quartz-ceramics are to prepare high speed high-altitude missile radome/antenna windows one of candidate material, with good high temperature power
Performance and dielectric properties are learned, manufacturing process is relatively easy, has the case of successful application, such as " patriot ", " Pan in the U.S.
It is emerging " No. two, " Aspide " guided missile of Italy etc., also reference can be made to [the wave transparent mechanism of silica system electromagnetic wave transparent material and research
Status _ Hao Hongshun].Meanwhile Al2O3Whisker is the splendid ceramic material of a kind of high temperature resistant, mechanical property.In fused quartz ceramic
In Al is added in a manner of growth in situ2O3Whisker can effectively improve the mechanical property and thermal shock resistance of ceramic material.
With the raising of aircraft speed, the reentry velocity of tactical missile especially of new generation is right up to tens Mach
Radome/antenna windows performance requirement is higher and higher, the mechanical property and thermal shock resistance of fused quartz ceramic need into
One step improves.
Summary of the invention
In order to solve the above-mentioned mechanical property that fused quartz ceramic how is improved when preparing radome/antenna windows and
The technical issues of thermal shock resistance, the present invention provides a kind of growth in situ alumina whiskers to enhance vitreous silica radar antenna
Cover/antenna windows preparation method, specific step is as follows for this method:
Step 1: mixed solution 1 and white powder substance 1 are prepared
Moderate amount of sulfuric acid aluminum solutions are taken at room temperature, and hexamethylene diamine is added thereto and makees template, uniform stirring obtains mixed solution 1;
Mixed solution 1 is placed in Muffle furnace, 160-180 DEG C is warming up to the rate of 1-2 DEG C/min, keeps the temperature 18-24 hours, took out
Filter, 80 DEG C of filter residue drying, obtains white powder substance 1;
Step 2: sol solution is prepared
It takes appropriate PVAC polyvinylalcohol to be placed in a beaker, deionized water is added, heating stirring to polyvinyl alcohol is completely dissolved
Sol solution, wherein PVAC polyvinylalcohol and the mass ratio of deionized water are 1:16-20, and heating temperature is 70-80 DEG C, stirring rate
For 80-100r/min;
Step 3: powdered rubber 2 is prepared
Appropriate yttrium oxide, white powder substance 1, vitreous silica is taken to be placed in sol solution obtained by step 2, the side Bian Jiare
Ultrasonic vibration, until moisture evaporates;Then mixture is dried, ball milling 24-48 hours under air environment, crosses 800-1000 mesh
Obtain powdered rubber 2;
Step 4: demoulding prod is prepared
Powdered rubber 2 obtained by step 3 is placed in radome/antenna windows mold, 90-120 DEG C is forced into 5-
10MPa pressure maintaining 4-6 hours, cools to room temperature with the furnace, takes out, and demoulding obtains demoulding prod;
Step 5: preform is obtained
Demoulding prod obtained by step 4 is placed in vacuum sintering funace, is passed through nitrogen or argon gas, flow 100-
200ml/min, heating and thermal insulation for a period of time after, be slowly dropped to room temperature, take out preform.
Step 6: post-processing obtains finished product
Flash is modified according to size, obtains finished product radome/antenna windows.
As an improvement, the mass ratio of aluminum sulfate and ethylenediamine is 1:(8-12 in step 1).
As an improvement, heating temperature is 70-80 DEG C, stirring rate 200-400r/min in step 3;Aoxidize yttrium powder
End, PVA, white powder substance 1 and vitreous silica mass ratio be (1-2): (5-10): (5-20): 100.
As an improvement, be industrial standard by nitrogen or argon gas in step 5, pressure 10-15MPa is kept, 6-8 hours
It is slowly heated to 1200-1400 DEG C of heat preservation 10-12 hours, subsequent 8-10 hours is slowly dropped to room temperature, takes out preform.
Meanwhile additionally providing the radome/antenna windows produced using above-mentioned preparation method.
The utility model has the advantages that growth in situ alumina whisker provided by the invention enhances vitreous silica radome/antenna windows
Preparation method, be by using aluminum sulfate as raw material, hexamethylene diamine is model agent, and preparing has specific molecular structure guiding
Al2O3Powder.Introduce yttrium oxide powder as sintering aid, at high temperature with Al2O3Solid solution is formed, in-situ preparation is promoted
Al2O3Whisker.Al2O3Whisker large specific surface area, itself has high mechanical property.As reinforcing material, can effectively increase
With the contact area of vitreous silica, the interfacial combined function of reinforcement and ceramic matrix is improved.Under high-temperature work environment, Al2O3
Whisker performance is stablized, and plays the role of bridging matrix micro-cracks, improves radome/antenna windows high-temperature behavior and anti-thermal shock
Performance.
Radome/antenna windows of this method preparation, dielectric constant is 2.5- under tensile strength > 150MPa, 10GHz
4.0, dielectric loss 0.005-0.020.1000 DEG C of 6 as a child tensile strength retention rate > 85% of work, meet high-speed aircraft
To radome/antenna windows use demand.
Specific embodiment
The present invention is further illustrated in conjunction with the embodiments below.
Embodiment one:
Step 1: taking the aluminum sulfate solution of 1000ml concentration 0.1mol/L at room temperature, and 300g hexamethylene diamine is added thereto and makees
Template, uniform stirring obtain mixed solution 1.Mixed solution 1 is placed in Muffle furnace, is warming up to 160 with the rate of 1 DEG C/min
DEG C, 18 hours are kept the temperature, filtering is taken out, 80 DEG C of filter residue drying obtain white powder substance 1.
Step 2: taking 5g polyvinyl alcohol (PVA) to be placed in a beaker, and 100g deionized water, heating stirring to polyethylene is added
Alcohol is completely dissolved to obtain sol solution.Wherein, heating temperature is 70 DEG C, stirring rate 100r/min.
Step 3: 1g yttrium oxide powder, 5g white powder substance 1 and 100g vitreous silica are placed in glue obtained by step 2
In solution, the side Bian Jiare ultrasonic vibration, until moisture evaporates.Wherein, heating temperature is 80 DEG C, stirring rate 200r/min.With
Mixture is dried afterwards, ball milling 24 hours under air environment, crosses 800 meshes, obtain powdered rubber 2.
Step 4: powdered rubber 2 obtained by step 3 is placed in radome mold, 90 DEG C are forced into 5MPa, pressure maintaining 4
Hour, cool to room temperature with the furnace.It takes out, demoulding.
Step 5: demoulding prod obtained by step 4 is placed in vacuum sintering funace, is passed through nitrogen, flow 100ml/
min.Nitrogen is industrial standard.Pressure 15MPa is kept, 1200 DEG C is slowly heated within 8 hours and keeps the temperature 12 hours, subsequent 8 hours slow
Slowly it is down to room temperature, taken out.
Step 6: flash is modified according to size, obtains radome.
The radome of this method preparation, dielectric constant is 3.3 under tensile strength 182MPa, 10GHz, dielectric loss
0.013.As a child tensile strength retention rate is 87% for 1000 DEG C of work 6, meets use of the high-speed aircraft to radome
Demand.
Reverse side embodiment one:
Step 1: taking the aluminum sulfate solution of 1000ml concentration 0.1mol/L at room temperature, and 300g hexamethylene diamine is added thereto and makees
Template, uniform stirring obtain mixed solution 1.Mixed solution 1 is placed in Muffle furnace, is warming up to 160 with the rate of 1 DEG C/min
DEG C, 18 hours are kept the temperature, filtering is taken out, 80 DEG C of filter residue drying obtain white powder substance 1.
Step 2: taking 5g polyvinyl alcohol (PVA) to be placed in a beaker, and 100g deionized water, heating stirring to polyethylene is added
Alcohol is completely dissolved to obtain sol solution.Wherein, heating temperature is 70 DEG C, stirring rate 100r/min.
Step 3: 5g white powder substance 1 and 100g vitreous silica are placed in sol solution obtained by step 2, Bian Jiare
Side ultrasonic vibration, until moisture evaporates.Wherein, heating temperature is 80 DEG C, stirring rate 200r/min.Then by mixture in sky
Compression ring is dried under border, ball milling 24 hours, is crossed 800 meshes, is obtained powdered rubber 2.
Step 4: powdered rubber 2 obtained by step 3 is placed in radome mold, 90 DEG C are forced into 5MPa, pressure maintaining 4
Hour, cool to room temperature with the furnace.It takes out, demoulding.
Step 5: demoulding prod obtained by step 4 is placed in vacuum sintering funace, is passed through nitrogen, flow 100ml/
min.Nitrogen is industrial standard.Pressure 15MPa is kept, 1200 DEG C is slowly heated within 8 hours and keeps the temperature 12 hours, subsequent 8 hours slow
Slowly it is down to room temperature, taken out.
Step 6: flash is modified according to size, obtains radome.
The reverse side embodiment and the difference of embodiment one are, do not add yttrium oxide as sintering aid.
The radome of this method preparation, tensile strength only 163Mpa, it is seen that sintering character is substantially reduced.
Embodiment two:
Step 1: taking the aluminum sulfate solution of 500ml concentration 0.15mol/L at room temperature, and 250g hexamethylene diamine is added thereto and makees
Template, uniform stirring obtain mixed solution 1.Mixed solution 1 is placed in Muffle furnace, is warming up to 180 with the rate of 2 DEG C/min
DEG C, 24 hours are kept the temperature, filtering is taken out, 80 DEG C of filter residue drying obtain white powder substance 1.
Step 2: taking 10g polyvinyl alcohol (PVA) to be placed in a beaker, and 100g deionized water, heating stirring to polyethylene is added
Alcohol is completely dissolved to obtain sol solution.Wherein, heating temperature is 70 DEG C, stirring rate 80r/min.
Step 3: 2g yttrium oxide powder, 10g white powder substance 1 and 100g vitreous silica are placed in obtained by step 2
In sol solution, the side Bian Jiare ultrasonic vibration, until moisture evaporates.Wherein, heating temperature is 80 DEG C, stirring rate 200r/min.
Then mixture is dried, ball milling 30 hours under air environment, crosses 1000 meshes, obtain powdered rubber 2.
Step 4: powdered rubber 2 obtained by step 3 is placed in radar antenna window mold, and 120 DEG C are forced into 10MPa, is protected
Pressure 6 hours, cools to room temperature with the furnace.It takes out, demoulding.
Step 5: demoulding prod obtained by step 4 is placed in vacuum sintering funace, is passed through argon gas, flow 200ml/
min.Argon gas is industrial standard.Pressure 12MPa is kept, 1400 DEG C is slowly heated within 8 hours and keeps the temperature 12 hours, subsequent 10 hours slow
Slowly it is down to room temperature, taken out.
Step 6: flash is modified according to size, obtains radar antenna window.
The radar antenna window of this method preparation, dielectric constant is 3.8 under tensile strength 203MPa, 10GHz, dielectric loss
0.018.1000 DEG C of 6 as a child tensile strength retention rates 91% of work, meet high-speed aircraft to the use need of radar antenna window
It asks.
Reverse side embodiment two:
Step 1: taking the aluminum sulfate solution of 500ml concentration 0.15mol/L at room temperature, and 250g hexamethylene diamine is added thereto and makees
Template, uniform stirring obtain mixed solution 1.Mixed solution 1 is placed in Muffle furnace, is warming up to 180 with the rate of 2 DEG C/min
DEG C, 24 hours are kept the temperature, filtering is taken out, 80 DEG C of filter residue drying obtain white powder substance 1.
Step 2: 2g yttrium oxide powder, 10g white powder substance 1 and 100g vitreous silica are placed in aqueous solution, side
Side ultrasonic vibration is heated, until moisture evaporates.Wherein, heating temperature is 80 DEG C, stirring rate 200r/min.Then by mixture
It is dried under air environment, crosses 1000 meshes, obtain powdered rubber 2.
Step 3: powdered rubber 2 obtained by step 3 is placed in radar antenna window mold, and 120 DEG C are forced into 10MPa, is protected
Pressure 6 hours, cools to room temperature with the furnace.It takes out, demoulding.
Step 4: demoulding prod obtained by step 4 is placed in vacuum sintering funace, is passed through argon gas, flow 200ml/
min.Argon gas is industrial standard.Pressure 12MPa is kept, 1400 DEG C is slowly heated within 8 hours and keeps the temperature 12 hours, subsequent 10 hours slow
Slowly it is down to room temperature, taken out.
Step 5: flash is modified according to size, obtains radar antenna window.
The reverse side embodiment and the difference of embodiment two are: yttrium oxide powder, white powder substance 1 and vitreous silica
It is placed in aqueous solution, rather than the sol solution of PVA.Powder is caused to be easy agglomerating and sink to the bottom, dispersion performance is greatly reduced.
The radar antenna window of this method preparation, dielectric constant is 3.9 under tensile strength 151MPa, 10GHz, dielectric loss
0.016.1000 DEG C of 6 as a child tensile strength retention rates 82% of work.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (5)
1. a kind of growth in situ alumina whisker enhances vitreous silica radome/antenna windows preparation method, feature exists
In specific step is as follows for this method:
Step 1: mixed solution 1 and white powder substance 1 are prepared
Moderate amount of sulfuric acid aluminum solutions are taken at room temperature, and hexamethylene diamine is added thereto and makees template, uniform stirring obtains mixed solution 1;It will mix
It closes solution 1 to be placed in Muffle furnace, is warming up to 160-180 DEG C with the rate of 1-2 DEG C/min, keeps the temperature 18-24 hours, take out filtering,
80 DEG C of filter residue drying, obtain white powder substance 1;
Step 2: sol solution is prepared
It takes appropriate PVAC polyvinylalcohol to be placed in a beaker, deionized water is added, heating stirring to polyvinyl alcohol is completely dissolved to obtain peptization
Liquid, wherein PVAC polyvinylalcohol and the mass ratio of deionized water are 1:(16-20), heating temperature is 70-80 DEG C, and stirring rate is
80-100r/min;
Step 3: powdered rubber 2 is prepared
Appropriate yttrium oxide, white powder substance 1, vitreous silica is taken to be placed in sol solution obtained by step 2, the side Bian Jiare ultrasound
Concussion, until moisture evaporates;Then mixture is dried, ball milling 24-48 hours under air environment, crosses 800-1000 mesh and obtain powder
Last substance 2;
Step 4: demoulding prod is prepared
Powdered rubber 2 obtained by step 3 is placed in radome/antenna windows mold, 90-120 DEG C is forced into 5-10MPa, protects
Pressure 4-6 hours, cools to room temperature with the furnace, takes out, and demoulding obtains demoulding prod;
Step 5: preform is obtained
Demoulding prod obtained by step 4 is placed in vacuum sintering funace, is passed through nitrogen or argon gas, flow 100-200ml/
Min, heating and thermal insulation for a period of time after, be slowly dropped to room temperature, take out preform.
Step 6: post-processing obtains finished product
Flash is modified according to size, obtains finished product radome/antenna windows.
2. growth in situ alumina whisker according to claim 1 enhances vitreous silica radome/antenna windows system
Preparation Method, which is characterized in that in step 1, the mass ratio of aluminum sulfate and ethylenediamine is 1:(8-12).
3. growth in situ alumina whisker according to claim 1 enhances vitreous silica radome/antenna windows system
Preparation Method, which is characterized in that in step 3, heating temperature is 70-80 DEG C, stirring rate 200-400r/min;Aoxidize yttrium powder
End, PVA, white powder substance 1 and vitreous silica mass ratio be (1-2): (5-10): (5-20): 100.
4. growth in situ alumina whisker according to claim 1 enhances vitreous silica radome/antenna windows system
Preparation Method, which is characterized in that be industrial standard by nitrogen or argon gas in step 5, keep pressure 10-15MPa, 6-8 is small
When be slowly heated to 1200-1400 DEG C of heat preservation 10-12 hours, subsequent 8-10 hours is slowly dropped to room temperature, takes out preform.
5. a kind of any one of -4 growth in situ alumina whisker enhancing vitreous silica radome according to claim 1/
Radome/antenna windows of the preparation method production of antenna windows.
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US20050133963A1 (en) * | 2003-12-18 | 2005-06-23 | The Regents Of The University Of California, A California Corporation | Silicon carbide whisker-reinforced ceramics with low rate of grain size increase upon densification |
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2019
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