CN102276278B - Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material - Google Patents
Preparation method of inorganic composite coating on surface of silica fiber-reinforced silica-based composite material Download PDFInfo
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Abstract
The invention which belongs to the technical field of special functional ceramic materials relates to a preparation method of an inorganic composite coating on the surface of a silica fiber-reinforced silica-based composite material. The preparation method comprises procedures of surface treatment, coating slurry preparation, spray, thermal treatment, and coating with a material for modification, wherein the temperature of the thermal treatment is 500-650DEG C. According to the invention, a solid phase reaction is carried out on three substances of lithium carbonate, aluminum hydroxide, and silica when being calcined, and a low expansion ceramic material is prepared by controlling the ratio among the three substances; a borate or a phosphate and the like are simultaneously introduced to prepare a low temperature flux to reduce the melting temperature of the integral body of the low expansion ceramic material; and a solidification hydrolysis reaction is finally carried out on an inorganic silicone resin to form a compact protection layer on the surface of a transition layer to reach effects of modification and double layer protection. The preparation method of the invention is scientific and reasonable, and is easy to implement, the material of the inorganic composite coating obtained with the preparation method has a good moistureproof performance, and has a good physicochemical match with the silica fiber-reinforced silica-based composite material, and simultaneously can improve dielectric properties of the silica fiber-reinforced silica-based composite material.
Description
Technical field
The invention belongs to special type, technical field of functional ceramics, relate to the preparation method that a kind of silica fiber strengthens silica based composite material surface inorganic composite coating.
Background technology
The continuous development of aeronautical and space technology has also proposed increasingly high requirement to the performance of electromagnetic wave transparent material; The stupalith of one-component can't satisfy working conditions because of itself inherent shortcoming (low like toughness, fragility is big etc.), so the inorganic fibre fabric composite study has become a kind of inevitable trend.Fiber as reinforced fabric mainly contains silica fiber, sapphire whisker and boron nitride fibre etc. at present, and their matrix material is used widely in multinomial Aeronautics and Astronautics engineering parts such as nose cone, heat-protection layer, antenna windows, radome successively.
Silica fiber strengthens the fragility that the silica based matrix material has overcome the simple substance pottery, has high toughness, has a wide range of applications in field of aerospace.But the goods void content is higher, not fine and close, surface hardness is lower, the scouring capability of in use bearing weathering and air-flow is relatively poor, thereby causes surface erosion, makes the surface coarse damage that becomes.The goods meeting moisture absorption in the prolonged preservation process causes wave penetrate capability to degenerate simultaneously.Therefore, the surface must apply floor height inorganic coating fine and close, that do not absorb water and could guarantee that matrix material has the advantages of high practicability ability.
Simultaneously; Because the silica fiber in the silica fiber matrix material is when handling down greater than 700 ℃; Its intensity will descend significantly; Cause silica fiber not have the enhanced effect, therefore the inorganic composite coating material of development should possess following condition: 1. be lower than 650 ℃ and can form the dense coating that does not absorb water down; 2. because the silica fiber enhancing silica based matrix material coefficient of expansion is extremely low, surface smoothness is relatively poor, so each item physical and chemical performance that is complementary must be arranged; 3. surperficial high densification and water-intake rate are zero.
Summary of the invention
The object of the present invention is to provide a kind of silica fiber to strengthen the preparation method of silica based composite material surface inorganic composite coating, its thermal treatment temp is lower than 650 ℃, and can form the dense coating that does not absorb water; The inorganic composite coating material moisture performance that obtains is good, not only with matrix good physical chemistry matching is arranged, and with matrix higher binding strength is arranged, and can improve the dielectric properties of material.
Silica fiber of the present invention strengthens the preparation method of silica based composite material surface inorganic composite coating, may further comprise the steps:
(1) surface treatment: handle on the surface that silica fiber is strengthened the silica based matrix material;
(2) coating slip preparation: primer, surface material are mixed with bottom slip and surface layer slip with organic binder bond and deionized water respectively;
(3) spraying: carry out drying treatment after bottom slip and surface layer slip be sprayed on silica fiber enhancing silica based composite material surface successively;
(4) thermal treatment: dried surface is heat-treated under 500～650 ℃;
(5) apply the curing decorative material: the coatingsurface after thermal treatment applies decorative material, behind 130～260 ℃ of baking-curings, makes inorganic composite coating.
Described organic binder bond is methylated cellulose aqueous solution or polyvinyl alcohol water solution, and strength of solution is 0.15～1.5%.
Described primer is founded at 1000～1200 ℃ after mixing, the shrend after drying, is pulverized and to make by the following batching of forming, and the percentage composition of batching quality is: Quilonum Retard 8～37%, boric acid 9～54%, white lake 11～24%, quartzy 17～30%, titanium oxide 0.1～0.7%, zirconium white 0.1～1%, White tin oxide 0.1～7%, lanthanum trioxide 0.1～4%, secondary calcium phosphate 0.3～10% and Sellaite 0.1～5%.
The ingredient groups of described bottom slip becomes: the primer quality: the organic binder bond volume: the ratio of deionized water volume is 10: 7～10: 3～7.
Described surface material is founded at 850～1100 ℃ after mixing, the shrend after drying, is pulverized and to make by the following batching of forming, and the percentage composition of batching quality is: Quilonum Retard 6～40%, white lake 10～37%, quartzy 7～35%, boric acid 13～68%, Natural manganese dioxide 0.2～5%, titanium oxide 0.2～3% and zinc oxide 0.3～10%.
The ingredient groups of described surface layer slip becomes: the surface material quality: the organic binder bond volume: the ratio of deionized water volume is 10: 4～9: 3～8.
Described decorative material is to be the batch mixes of inorganic polysiloxane 40～80% and solidifying agent 20～60% with the quality percentage composition, stirs 3～20 hours, obtains to water white transparency.
The raw material specification of using in the above-mentioned prescription is following:
Quilonum Retard weight content >=99.0%; The weight content of boric acid >=99.5%; White lake is AR; Natural manganese dioxide is lightweight, its weight content >=98.5%; Zirconium white weight content >=99.0%; Zinc oxide weight content >=99.5%; Sellaite weight content >=99.0%; White tin oxide weight content >=99.0%; Lanthanum trioxide weight content >=99.0%; Secondary calcium phosphate weight content >=99.0%; Quartz is an amorphous state, silica weight content >=99.98%; Titanium oxide, CP, weight content >=98%.
The present invention prepares in the process, the surface treatment of employing, spraying, drying, thermal treatment, solidifies, founds and steps such as shrend, is techniques well known.
The present invention utilizes Quilonum Retard, white lake and silicon-dioxide three that solid state reaction takes place under high-temperature calcination, prepares expansion ceramic material through controlling triangular ratio; Introduce the melt temperature of preparation low temperature fusing assistants such as borate or phosphoric acid salt simultaneously, thereby make coating required under the low temperature with the reduction material monolithic; Utilize the curing hydrolysis of inorganic polysiloxane to be reflected at the finer and close resist of transition layer surface formation one deck at last, reach the effect of modification and double shielding.
Beneficial effect of the present invention is following:
The present invention is scientific and reasonable, and is easy to implement, and the inorganic composite coating material moisture performance of acquisition is good; Strengthen the silica based matrix material with silica fiber good physical chemistry matching is arranged; Good with matrix bond property, can improve the dielectric properties of material, also have good shock resistance simultaneously.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1
1, the preparation of coated material
(1) preparation of primer: take by weighing Quilonum Retard 100g, boric acid 240g, white lake 95g, quartzy 135g, titanium oxide 1g, zirconium white 1g, White tin oxide 1.5g, lanthanum trioxide 0.75g, secondary calcium phosphate 40g and Sellaite 15g; Mix; Place Cinker clew furnace to found for 1150 ℃, shrend after drying, pulverizing make.
(2) preparation of surface material: take by weighing Quilonum Retard 90g, white lake 75g, quartzy 75g, boric acid 250g, Natural manganese dioxide 5g, titanium oxide 5g and zinc oxide 25g, mix, place Cinker clew furnace under 900 ℃, to found, shrend after drying, pulverizing make.
2, the preparation of decorative material
Take by weighing inorganic polysiloxane 70g, solidifying agent 30g, stirred 6 hours, make to water white transparency.
3, the preparation of compound coating
(1) surface treatment: handle on the surface that silica fiber is strengthened the silica based matrix material;
(2) coating slip preparation: take by weighing primer 10g, with 8ml concentration be that 0.3% methylated cellulose aqueous solution and 5ml deionized water are made into the bottom slip, ball milling 0.5h mixing;
Take by weighing surface material 10g equally, with 6ml concentration be that 0.3% methylated cellulose aqueous solution and 6ml deionized water are made into the surface layer slip, ball milling 0.5h mixing.
(3) spraying: spray the bottom slip earlier, control thickness is about 0.15mm; And then spraying surface layer slip, gauge control places 80 ℃ of baking ovens dry about 0.1mm.
(4) thermal treatment: after the drying, under 600 ℃, heat-treat;
(5) apply the curing decorative material: the coatingsurface after thermal treatment applies decorative material, and gauge control through 160 ℃ of baking-curings, makes inorganic composite coating about 0.1mm.
This compound coating and matrix have associativity preferably, flawless, do not absorb water.600 ℃, 800 ℃, 1000 ℃ each chillings three times, coating does not ftracture, does not peel off with the inorganic composite coating for preparing.
Embodiment 2
1, the preparation of coated material
(1) preparation of primer: take by weighing Quilonum Retard 83g, boric acid 220g, white lake 80g, quartzy 150g, titanium oxide 1g, zirconium white 1g, White tin oxide 3.5g, lanthanum trioxide 1g, secondary calcium phosphate 18g and Sellaite 8g; Mix; Place Cinker clew furnace to found for 1200 ℃, shrend after drying, pulverizing make.
(2) preparation of surface material: take by weighing Quilonum Retard 114g, white lake 63g, quartzy 60g, boric acid 300g, Natural manganese dioxide 7g, titanium oxide 7g and zinc oxide 18g, mix, place Cinker clew furnace under 1000 ℃, to found, shrend after drying, pulverizing make.
2, the preparation of decorative material
Take by weighing inorganic polysiloxane 30g, solidifying agent 15g, stirred 12 hours, make to water white transparency.
3, the preparation of compound coating
(1) surface treatment: handle on the surface that silica fiber is strengthened the silica based matrix material;
(2) coating slip preparation: take by weighing primer 10g, with 9ml concentration be that 1% polyvinyl alcohol water solution and 5ml deionized water are made into the bottom slip, ball milling 0.5h mixing.
Take by weighing surface material 10g equally, with 7ml concentration be that 1% polyvinyl alcohol water solution and 5ml deionized water are made into the surface layer slip, ball milling 0.5h mixing.
(3) spraying: spray the bottom slip earlier, control thickness is about 0.15mm; And then spraying surface layer slip, gauge control places 80 ℃ of baking ovens dry about 0.1mm;
(4) thermal treatment: after the drying, under 620 ℃, heat-treat;
(5) apply the curing decorative material: the coatingsurface after thermal treatment applies decorative material, and gauge control through 230 ℃ of baking-curings, makes inorganic composite coating about 0.1mm.
This compound coating and matrix have associativity preferably, flawless, do not absorb water.600 ℃, 800 ℃, 1000 ℃ each chillings three times, coating does not ftracture, does not peel off with the inorganic composite coating for preparing.
Embodiment 3
1, the preparation of coated material
(1) preparation of primer: take by weighing Quilonum Retard 125g, boric acid 200g, white lake 65g, quartzy 100g, titanium oxide 1g, zirconium white 1.5g, White tin oxide 1.4g, lanthanum trioxide 1.5g, secondary calcium phosphate 3g and Sellaite 1.6g; Mix; Place Cinker clew furnace to found for 1050 ℃, shrend after drying, pulverizing make.
(2) preparation of surface material: take by weighing Quilonum Retard 40g, white lake 40g, quartzy 18g, boric acid 100g, Natural manganese dioxide 0.6g, titanium oxide 0.4g and zinc oxide 1g, mix, place Cinker clew furnace under 900 ℃, to found, shrend after drying, pulverizing make.
2, the preparation of decorative material
Take by weighing inorganic polysiloxane 30g, solidifying agent 30g, stirred 8 hours, make to water white transparency.
3, the preparation of compound coating
(1) surface treatment: handle on the surface that silica fiber is strengthened the silica based matrix material;
(2) coating slip preparation: take by weighing primer 10g, with 7ml concentration be that 0.3% methylated cellulose aqueous solution and 6ml deionized water are made into the bottom slip, ball milling 0.5h mixing;
Take by weighing surface material 10g equally, with 6ml concentration be that 0.3% methylated cellulose aqueous solution and 8ml deionized water are made into the surface layer slip, ball milling 0.5h mixing.
(3) spraying: spray the bottom slip earlier, control thickness is about 0.15mm; And then spraying surface layer slip, gauge control places 80 ℃ of baking ovens dry about 0.1mm.
(4) thermal treatment: after the drying, under 600 ℃, heat-treat;
(5) apply the curing decorative material: the coatingsurface after thermal treatment applies decorative material, and gauge control through 160 ℃ of baking-curings, makes inorganic composite coating about 0.1mm.
This compound coating and matrix have associativity preferably, flawless, do not absorb water.600 ℃, 800 ℃, 1000 ℃ each chillings three times, coating does not ftracture, does not peel off with the inorganic composite coating for preparing.
Embodiment 4
1, the preparation of coated material
(1) preparation of primer: take by weighing Quilonum Retard 160g, boric acid 115g, white lake 70g, quartzy 125g, titanium oxide 1.9g, zirconium white 2.5g, White tin oxide 7.5g, lanthanum trioxide 0.6g, secondary calcium phosphate 7.5g and Sellaite 10g; Mix; Place Cinker clew furnace to found for 1200 ℃, shrend after drying, pulverizing make.
(2) preparation of surface material: take by weighing Quilonum Retard 20g, white lake 36g, quartzy 20g, boric acid 120g, Natural manganese dioxide 0.8g, titanium oxide 1.6g and zinc oxide 1.6g, mix, place Cinker clew furnace under 1050 ℃, to found, shrend after drying, pulverizing make.
2, the preparation of decorative material
Take by weighing inorganic polysiloxane 30g, solidifying agent 15g, stirred 20 hours, make to water white transparency.
3, the preparation of compound coating
(1) surface treatment: handle on the surface that silica fiber is strengthened the silica based matrix material;
(2) coating slip preparation: take by weighing primer 10g, with 8.5ml concentration be that 1% polyvinyl alcohol water solution and 6.3ml deionized water are made into the bottom slip, ball milling 0.5h mixing.
Take by weighing surface material 10g equally, with 8ml concentration be that 1% polyvinyl alcohol water solution and 5.5ml deionized water are made into the surface layer slip, ball milling 0.5h mixing.
(3) spraying: spray the bottom slip earlier, control thickness is about 0.15mm; And then spraying surface layer slip, gauge control places 80 ℃ of baking ovens dry about 0.1mm;
(4) thermal treatment: after the drying, under 650 ℃, heat-treat;
(5) apply the curing decorative material: the coatingsurface after thermal treatment applies decorative material, and gauge control through 200 ℃ of baking-curings, makes inorganic composite coating about 0.1mm.
This compound coating and matrix have associativity preferably, flawless, do not absorb water.600 ℃, 800 ℃, 1000 ℃ each chillings three times, coating does not ftracture, does not peel off with the inorganic composite coating for preparing.
Claims (5)
1. a silica fiber strengthens the preparation method of silica based composite material surface inorganic composite coating, it is characterized in that may further comprise the steps:
(1) surface treatment: handle on the surface that silica fiber is strengthened the silica based matrix material;
(2) coating slip preparation: primer, surface material are mixed with bottom slip and surface layer slip with organic binder bond and deionized water respectively;
(3) spraying: carry out drying treatment after bottom slip and surface layer slip be sprayed on silica fiber enhancing silica based composite material surface successively;
(4) thermal treatment: dried surface is heat-treated under 500 ~ 650 ℃;
(5) apply the curing decorative material: the coatingsurface after thermal treatment applies decorative material, behind 130 ~ 260 ℃ of baking-curings, makes inorganic composite coating;
Primer is founded at 1000 ~ 1200 ℃ after mixing, the shrend after drying, is pulverized and to make by the following batching of forming, and the percentage composition of batching quality is: Quilonum Retard 8 ~ 37%, boric acid 9 ~ 54%, white lake 11 ~ 24%, quartzy 17 ~ 30%, titanium oxide 0.1 ~ 0.7%, zirconium white 0.1 ~ 1%, White tin oxide 0.1 ~ 7%, lanthanum trioxide 0.1 ~ 4%, secondary calcium phosphate 0.3 ~ 10% and Sellaite 0.1 ~ 5%;
Surface material is founded at 850 ~ 1100 ℃ after mixing, the shrend after drying, is pulverized and to make by the following batching of forming, and the percentage composition of batching quality is: Quilonum Retard 6 ~ 40%, white lake 10 ~ 37%, quartzy 7 ~ 35%, boric acid 13 ~ 68%, Natural manganese dioxide 0.2 ~ 5%, titanium oxide 0.2 ~ 3% and zinc oxide 0.3 ~ 10%.
2. silica fiber according to claim 1 strengthens the preparation method of silica based composite material surface inorganic composite coating, it is characterized in that organic binder bond is methylated cellulose aqueous solution or polyvinyl alcohol water solution, and strength of solution is 0.15 ~ 1.5%.
3. silica fiber according to claim 1 and 2 strengthens the preparation method of silica based composite material surface inorganic composite coating, and it is characterized in that the ingredient groups of bottom slip becomes: the primer quality: the organic binder bond volume: the ratio of deionized water volume is 10:7 ~ 10:3 ~ 7.
4. silica fiber according to claim 1 and 2 strengthens the preparation method of silica based composite material surface inorganic composite coating, and it is characterized in that the ingredient groups of surface layer slip becomes: the surface material quality: the organic binder bond volume: the ratio of deionized water volume is 10:4 ~ 9:3 ~ 8.
5. silica fiber according to claim 1 and 2 strengthens the preparation method of silica based composite material surface inorganic composite coating; It is characterized in that decorative material is is the batch mixes of inorganic polysiloxane 40 ~ 80% and solidifying agent 20 ~ 60% with the quality percentage composition; Stirred 3 ~ 20 hours, and obtained to water white transparency.
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| CN115231952B (en) * | 2022-07-15 | 2023-02-03 | 中国人民解放军国防科技大学 | Rain erosion resistant inorganic coating on surface of quartz fiber reinforced quartz-based composite material and preparation method thereof |
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| CN1236790A (en) * | 1999-04-02 | 1999-12-01 | 马玉通 | Electrothermal inorganic composite coating |
| CN101613209A (en) * | 2009-07-16 | 2009-12-30 | 中国人民解放军国防科学技术大学 | C fThe high-temperature oxidation resistant coating of/SiC matrix material, coating slurry and preparation method thereof |
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