CN102432324B - Preparation method of high-silica compound ceramic heat insulating product - Google Patents
Preparation method of high-silica compound ceramic heat insulating product Download PDFInfo
- Publication number
- CN102432324B CN102432324B CN 201110250629 CN201110250629A CN102432324B CN 102432324 B CN102432324 B CN 102432324B CN 201110250629 CN201110250629 CN 201110250629 CN 201110250629 A CN201110250629 A CN 201110250629A CN 102432324 B CN102432324 B CN 102432324B
- Authority
- CN
- China
- Prior art keywords
- high silica
- heat insulating
- silica fiber
- preparation
- silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses a preparation method of a high-silica compound ceramic heat insulating product. The method comprises the following steps of: (1) boiling high-silica fiber braided bodies with water in sequence, drying, introducing oxygen into a vacuum container for baking, washing with acid, washing with water and drying; (2) soaking the high-silica fiber braided bodies in silica sol for 30-60 minutes, and controlling the density of the silica sol at 1.12-1.16 g/cm<3>; (3) vibrating the silica sol, continually soaking the high-silica fiber braided bodies for 30-60 minutes, taking out, and drying for 20-40 hours; (4) repeatedly treating the high-silica fiber braided bodies according to the step (2) and step (3) for 2-6 times; (5) performing thermal treatment on the high-silica fiber braided bodies at the temperature of 300-700 DEG C till the high-silica fiber braided bodies become half-ceramic rough blanks; and (6) processing the rough blanks to the needed product size to obtain the high-silica compound ceramic heat insulating product. The preparation method has a simple process and is low in cost, and the obtained product has the characteristics of low heat conducting coefficient, good heat insulating effect, high mechanical property and superior thermal physical property.
Description
Technical field
The invention belongs to high silica composite ceramic material technical field, be specifically related to a kind of preparation method of high silica compound ceramic heat insulating product.
Technical background
Be arranged on high temperature resistant (〉=1000 ℃) insulation products of missile armament control cabinet outside, reentering, playing a part in process during motor-driven, long boat heat insulation, carrying and anti-ablation, can guarantee that in control cabinet, envrionment temperature remains in 200 ℃, ensure that in control cabinet, components and parts can work in abominable reentry environment.The technical development during to large range, large Mach, high motor-driven, long boat along with missile weapon system, easily very fast ablation under high-temperature condition, the heat insulation service requirements of control cabinet when the conventional resins base lagging material that vapors away can not satisfy long boat, thus high temperature ceramic material become essential.At present, the high temperature insulation thyrite that existing engineering is used exists thermal conductivity bigger than normal, is 14W/mk during room temperature to 300 ℃, and effect of heat insulation is relatively poor.And silicon carbide ceramics is extremely expensive with fiber and body material price, and carbon fiber (3K) market price is about 4500 yuan/kilogram, and approximately 6000 yuan/kilogram of polycarbosilane precusor market prices are high with the product cost of its making.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of technique high silica compound ceramic heat insulating product simple, with low cost.Adopt that product that the method makes has that thermal conductivity is low, good heat-insulation effect, mechanical property is strong, heat physical properties is excellent characteristic.
For achieving the above object, the preparation method of the high silica composite ceramics that the present invention is designed comprises the following steps:
1) first with high silica fiber knitted body logical oxygen roasting 1～3h, pickling, washing and drying and processing again in poach 20～40h, oven dry 10～15h, 250～500 ℃ of lower vacuum vessels successively;
2) secondly the fine knitted body of high silica is placed in silicon sol and floods 30～60min, the density of controlling described silicon sol is 1.12～1.16g/cm
3
3) then vibrate silicon sol, continue the fine knitted body 30～60min of the high silica of dipping, take out dry 20～40h;
4) again to the fine knitted body repeating step 2 of high silica) and step 3) processing mode 2～6 times;
5) then the fine knitted body of high silica is heat-treated, thermal treatment temp is controlled at 300～700 ℃, makes fine knitted body half pottery of high silica change into crude green body;
6) at last crude green body is processed into required product size, namely obtains high silica compound ceramic heat insulating product.
Further, described step 1) in, acid cleaning process is that to adopt volume ratio be that concentrated hydrochloric acid and the concentrated nitric acid mixed solution of 3: 1 washs.
Again further, described step 2) in, steeping process carries out in vacuum vessel.
Further, described step 5) in, thermal treatment temp is controlled at 400～500 ℃.
In the preparation method of the high silica compound ceramic heat insulating product of the present invention, each process parameter principle of qualification and advantage are as follows:
The present invention by poach, oven dry, roasting, pickling, washing and the measure pre-treatment such as oven dry again, has removed the treating compound on high silica fiber surface with the high silica fiber knitted body fully.Then adopt silicon sol to make matrix, the high silica fiber knitted body is carried out the dipping of for some time, make the silicon sol matrix effectively fill the gap of high silica fiber knitted body, strengthened the compactness of high silica fiber knitted body.Dipping preferably carries out under vacuum state, because under vacuum condition, the air in high silica fiber is drawn out of, and the quartz particles that more is conducive in silicon sol enters the gap, and filling effect is better.Vibrate dipping after common dipping, under the mechanical vibration effect, silicon sol is combined tightr with the high silica fiber knitted body again.In order to obtain better filling effect, common dipping and vibration dipping are repeated 2～6 times successively.Then to the high silica fiber knitted body drying dehydration after the vibration dip treating, silicon sol is solidified, again through 300～700 ℃ of low-temperature heat treatment, at this temperature, high silica fiber and silicon sol matrix material part crystalline phase, form half ceramic crude green body, the crude green body toughness of this half ceramic treatment is high, non-friable, and processes temperature required lowly, can reduce technology difficulty and production cost.At last, crude green body is machined into the desired product size, namely obtains high silica compound ceramic heat insulating product.
And, approximately 450 yuan/kilogram of the starting material high silica fiber market prices that preparation method of the present invention adopts, approximately 100 yuan/kilogram of silicon sol, with low cost, can big area use on engineering.The hot coefficient that obtained high silica composite ceramics is led insulation products is lower than 0.6W/mk (room temperature～300 ℃), and low more than silicon carbide ceramics, effect of heat insulation is better.The outer heat-insulating problem of control cabinet in missile armament flight course when product of the present invention can successfully solve large range, large Mach, high motor-driven, long boat.
Embodiment
Preparation method to the high silica compound ceramic heat insulating product of the present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
When making high silica composite ceramics thermal-insulated frame, according to the geometrical dimension requirement of designed thermal-insulated frame, be woven into profiling thermal-insulated frame structure with high silica fiber in advance, then:
1) first the high silica fiber thermal-insulated frame is placed in container poach 20h, oven dry 10h, logical oxygen roasting 1h under the vacuum state of 250 ℃ again, then adopting volume ratio is that concentrated hydrochloric acid and the concentrated nitric acid mixed solution of 3: 1 carries out cleanup acid treatment to it, after pickling, it is washed, dries.
2) secondly the high silica fiber thermal-insulated frame is placed in stainless steel cask and vacuumizes, and slowly suction density is 1.12g/cm
3Silicon sol flood the high silica fiber thermal-insulated frame, flood 30min in silicon sol.
3) then vibrate stainless steel cask, make silicon sol produce big ups and downs, continue to take out dry 20h after infiltration high silica fiber thermal-insulated frame 30min.
4) again to high silica fiber thermal-insulated frame repeating step 2) and step 3) processing mode 4 times.
5) then the high silica fiber thermal-insulated frame is heat-treated, thermal treatment temp is controlled at 400 ℃, makes high silica fiber thermal-insulated frame half pottery change into crude green body.
6) last double ceramic crude green body carries out the removal of impurity, is processed into the desired product size, namely makes high silica composite ceramics thermal-insulated frame product.
The high silica composite ceramics thermal-insulated frame product that adopts the inventive method to make, density is 1.54g/cm
3, thermal conductivity is 0.52W/mk (room temperature～300 ℃), and flexural strength is 25MPa, and linear ablative rate is 0.12mm/s, and property indices meets design requirement.
Embodiment 2
When making high silica composite ceramics thermal baffle, according to the geometrical dimension requirement of designed thermal baffle, be woven into the profiling heat insulation plate structure with high silica fiber in advance, then:
1) first the high silica fiber thermal baffle is placed in container poach 30h, oven dry 15h, logical oxygen roasting 2h under 500 ℃ of lower vacuum states again, then adopting volume ratio is that concentrated hydrochloric acid and the concentrated nitric acid mixed solution of 3: 1 carries out cleanup acid treatment to it, after pickling, it is washed, dries.
2) secondly the high silica fiber thermal baffle is placed in stainless steel cask and vacuumizes, and slowly suction density is 1.16g/cm
3Silicon sol floods the high silica fiber thermal baffle, floods 60min in silicon sol;
3) then vibrate stainless steel cask, make silicon sol produce big ups and downs, continue to take out dry 40h after infiltration high silica fiber thermal baffle 50min;
4) again to oxygen fiber thermal baffle repeating step 2) and step 3) processing mode 5 times;
5) then the high silica fiber thermal baffle is heat-treated, thermal treatment temp is controlled at 500 ℃, makes high silica fiber thermal baffle half pottery change into crude green body;
6) last double ceramic crude green body carries out the removal of impurity, is processed into the desired product size, namely makes high silica composite ceramics thermal baffle product.
The high silica composite ceramics thermal baffle product that adopts the inventive method to make, density is 1.56g/cm
3, thermal conductivity is 0.55W/mk (room temperature～300 ℃), and flexural strength is 30MPa, and linear ablative rate is 0.16mm/s, and properties reaches advanced international level.
Embodiment 3
When making high silica composite ceramics thermal insulation tile, according to the geometrical dimension requirement of designed thermal insulation tile, be woven into profiling thermal insulation tile structure with high silica fiber in advance, then:
1) first the high silica fiber thermal insulation tile is placed in container poach 40h, oven dry 12h, logical oxygen roasting 3h under 300 ℃ of lower vacuum states again, then adopting volume ratio is that concentrated hydrochloric acid and the concentrated nitric acid mixed solution of 3: 1 carries out cleanup acid treatment to it, after pickling, it is washed, dries.
2) secondly the high silica fiber thermal insulation tile is placed in stainless steel cask and vacuumizes, and slowly suction density is 1.15g/cm
3Silicon sol floods the high silica fiber thermal insulation tile, floods 30min in silicon sol;
3) then vibrate stainless steel cask, make silicon sol produce big ups and downs, continue to take out dry 40h after infiltration high silica fiber thermal insulation tile 60min;
4) again to oxygen fiber thermal insulation tile repeating step 2) and step 3) twice of processing mode;
5) then the high silica fiber thermal insulation tile is heat-treated, thermal treatment temp is controlled at 300 ℃, makes high silica fiber thermal insulation tile half pottery change into crude green body;
6) last double ceramic crude green body carries out the removal of impurity, is processed into the desired product size, namely makes high silica composite ceramics thermal insulation tile product.
The high silica composite ceramics thermal insulation tile product that adopts the inventive method to make, density is 1.60g/cm
3, thermal conductivity is 0.58W/mk (room temperature～300 ℃), and flexural strength is 35MPa, and linear ablative rate is 0.20mm/s, and properties reaches advanced international level.
Embodiment 4
When making high silica fiber composite ceramics heat insulation cylinder, in advance according to designed heat insulation cylinder product geometrical dimension requirement, be woven into profiling heat insulation cylinder structure with high silica fiber, then:
1) first the high silica fiber heat insulation cylinder is placed in container poach 40h, oven dry 15h, logical oxygen roasting 3h under 450 ℃ of lower vacuum states again, then adopting volume ratio is that concentrated hydrochloric acid and the concentrated nitric acid mixed solution of 3: 1 carries out cleanup acid treatment to it, after pickling, it is washed, dries.
2) secondly the high silica fiber heat insulation cylinder is placed in stainless steel cask and vacuumizes, and slowly suction density is 1.16g/cm
3Silicon sol floods the high silica fiber heat insulation cylinder, floods 40min in silicon sol;
3) then vibrate stainless steel cask, make silicon sol produce big ups and downs, continue to take out dry 35h after infiltration high silica fiber heat insulation cylinder 60min;
4) again to oxygen fiber heat insulation cylinder repeating step 2) and step 3) processing mode six times;
5) then the high silica fiber heat insulation cylinder is heat-treated, thermal treatment temp is controlled at 700 ℃, makes high silica fiber heat insulation cylinder half pottery change into crude green body;
6) at last half ceramic crude green body is carried out the removal of impurity, be processed into the desired product size, namely make high silica composite ceramics every the cylinder product.
The high silica composite ceramics heat insulation cylinder product that adopts the inventive method to make, density is 1.63g/cm
3, thermal conductivity is 0.60W/mk (room temperature～300 ℃), and flexural strength is 32MPa, and linear ablative rate is 0.18mm/s, and properties reaches advanced international level.
Claims (3)
1. the preparation method of a high silica compound ceramic heat insulating product comprises the following steps:
1) first with high silica fiber knitted body logical oxygen roasting 1 ~ 3h, pickling, washing and drying and processing again in poach 20 ~ 40h, oven dry 10 ~ 15h, 250 ~ 500 ℃ of lower vacuum vessels successively;
2) secondly the fine knitted body of high silica is placed in silicon sol and floods 30 ~ 60min, the density of controlling described silicon sol is 1.12 ~ 1.16g/cm
3
3) then vibrate silicon sol, continue the fine knitted body 30 ~ 60min of the high silica of dipping, take out dry 20 ~ 40h;
4) again to the fine knitted body repeating step 2 of high silica) and the processing mode of step 3) 2 ~ 6 times;
5) then the fine knitted body of high silica is heat-treated, thermal treatment temp is controlled at 400 ~ 500 ℃, makes fine knitted body half pottery of high silica change into crude green body;
6) at last crude green body is processed into required product size, namely obtains high silica compound ceramic heat insulating product.
2. the preparation method of high silica compound ceramic heat insulating product according to claim 1 is characterized in that: in described step 1), acid cleaning process is that to adopt volume ratio be that concentrated hydrochloric acid and the concentrated nitric acid mixed solution of 3 ︰ 1 washs.
3. the preparation method of high silica compound ceramic heat insulating product according to claim 1 and 2, it is characterized in that: described step 2), steeping process carries out in vacuum vessel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110250629 CN102432324B (en) | 2011-08-29 | 2011-08-29 | Preparation method of high-silica compound ceramic heat insulating product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110250629 CN102432324B (en) | 2011-08-29 | 2011-08-29 | Preparation method of high-silica compound ceramic heat insulating product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102432324A CN102432324A (en) | 2012-05-02 |
| CN102432324B true CN102432324B (en) | 2013-06-26 |
Family
ID=45980720
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110250629 Expired - Fee Related CN102432324B (en) | 2011-08-29 | 2011-08-29 | Preparation method of high-silica compound ceramic heat insulating product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102432324B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860695B (en) * | 2015-04-30 | 2017-03-01 | 中国人民解放军国防科学技术大学 | Three-dimensional fiber prefabricated component strengthens mullite composite material and preparation method thereof |
| CN106145988B (en) * | 2016-06-29 | 2018-11-23 | 湖北三江航天江北机械工程有限公司 | Bilayer prevents the preparation method of heat-insulated wave-penetrating composite material structural member |
| CN106518126B (en) * | 2016-10-26 | 2019-02-26 | 湖北三江航天江北机械工程有限公司 | The preparation method of whisker reinforcement quartz composite ceramic wave-transparent material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328221C (en) * | 2005-10-27 | 2007-07-25 | 中材高新材料股份有限公司 | Reinforced ceramic penetrating wave material with inorganic fibre fabric and preparation process thereof |
-
2011
- 2011-08-29 CN CN 201110250629 patent/CN102432324B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102432324A (en) | 2012-05-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106478105B (en) | A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon | |
| CN102432324B (en) | Preparation method of high-silica compound ceramic heat insulating product | |
| CN105601192B (en) | Inorganic compounding hole-opening foaming core material of vacuum heat insulation plate and preparation method thereof | |
| CN101269981B (en) | Process for producing carbon/carbon heat insulation bottom board for high temperature furnace | |
| CN103265331B (en) | C/SiC/Na2SiO3 antioxidative compound coating suitable for graphite material and preparation method thereof | |
| CN103204693A (en) | Preparation method for short carbon fiber/silicon carbide composites | |
| CN106630983A (en) | Preparation method of heat protection/insulation integral antenna cover and mold thereof | |
| CN103395783A (en) | Preparation method and preparation equipment of activated carbon | |
| CN103538132B (en) | Method for directly carbonizing wet timber | |
| CN102731060A (en) | Preparation method for carbon fiber felt reinforced C-Al2O3 composite aerogel | |
| CN103045983A (en) | Preparation method of carbon fiber-based high-temperature heat-insulating material with surface tungsten coating | |
| CN104478475A (en) | High-temperature-resistant high-strength SiC clad carbon foam composite thermal insulating material and preparation method thereof | |
| CN101913897B (en) | Inner port for electro-thermal cooker and production method thereof | |
| CN103771426A (en) | Method for firing porous cristobalite at low temperature by adopting diatomite as raw material | |
| CN102617177A (en) | Manufacture method of boron nitride fabric reinforced silicon-boron-nitrogen ceramic-based composite material | |
| CN104892013A (en) | Method for preparing SiC-based composite material | |
| CN101302089A (en) | Preparation of heat-insulating energy-saving mortar containing phase-change material | |
| CN106517195A (en) | Method for preparing porous carbon from phosphate activated biomass and applying porous carbon to supercapacitors | |
| CN102199034B (en) | Method for preparing cordierite-based microwave dielectric ceramic material | |
| CN108794037A (en) | A kind of preparation method of Carbon foam heat-insulation composite material | |
| CN105924138A (en) | Preparation method of fine-aperture foamed ceramic | |
| CN206598435U (en) | It is a kind of be used to manufacturing compound Carbon fiber thermal insulation cylinder vacuumize shaped device | |
| CN104926349A (en) | Method and depositing furnace for rapidly depositing and preparing C/C composite material by direct heating method | |
| CN101165006B (en) | Solid-phase sintering silicon carbide ceramic surface corrosion method | |
| CN108610019A (en) | A method of preparing low unit weight, high-intensity heat insulating material using polishing ceramic waste residue |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130626 Termination date: 20210829 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |