CN104892006A - Phosphate-doped ceramic coating material and preparation method thereof - Google Patents
Phosphate-doped ceramic coating material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a phosphate-doped ceramic coating material. The problem to be solved in the invention is easy loss of a metal material in high-speed dust impact, damp-hot and corrosion environment, and the surface of the metal material is coated with a phosphate-doped ceramic material to protect the metal material to a certain degree in order to prolong the service life of the metal material. The phosphate-doped ceramic material is composed of an aluminum dihydrogen phosphate-chromium dihydrogen phosphate solution, a diluent and a ceramic component. The preparation method comprises the following steps: 1, preparing the aluminum dihydrogen phosphate-chromium dihydrogen phosphate solution; 2, preparing the diluent; 3, preparing the ceramic component; and 4, preparing the phosphate-doped ceramic coating material. The phosphate-doped ceramic coating material prepared in the invention has the advantages of good wear, corrosion and high temperature resistance, and certain bonding performance, and is mainly used in gas erosion protection of the metal material and other bondable materials.
Description
Technical field
The present invention relates to ceramic coated materials technical field, particularly relate to a kind of phosphoric acid salt doped ceramics coating material and preparation method thereof, be mainly used in wear-resisting, the corrosion-resistant and resistant to elevated temperatures protection of parts between pipeline in metallurgy, electric power, coal industry, burning.
Background technology
Along with the development of industrial technology, the industries such as metallurgy, electric power, coal also improve constantly the demand of power system, and the nervous and coal dust quality of coal supply declines, therefore for ensureing that working efficiency then needs to increase the amount of delivering coal of unit time, this can make the ash content that is mingled with in hot gas flow coal dust more, air-flow velocity is faster, in addition water and nitrogenous can be produced after coal combustion, sulfur-bearing, chloride corrosive gases such as grade, these all will cause metallic conduit, parts are waited to impact at high speed dust for a long time between burning, high temperature, moist, work under corrosive environment, accelerate the deterioration of material, cause booster, the problems such as shutdown, cause waste and the leeway of material, even life-threatening, the safety of property.
Therefore a kind of wear-resisting, corrosion-resistant, resistant to elevated temperatures phosphoric acid salt doped ceramics coated materials of design is at metal material surface, can the impact of the direct crevice corrosion gas of available protecting metal and high speed dust, thus extends the work-ing life of material.
Summary of the invention
The present invention impacts and the problem of easily loss under damp and hot, corrosive environment at high speed dust to solve metallic substance; and provide a kind of phosphoric acid salt doped ceramics coating material and preparation method thereof; by at metal material surface applying phosphate doped ceramics material; thus to metallic substance, there is certain provide protection, reach the object extending metallic substance work-ing life.
The present invention adopts following technical scheme:
Phosphoric acid salt doped ceramics coating material of the present invention is made up of aluminium dihydrogen phosphate-biphosphate chromium solution, thinner and ceramic composition, and its concrete weight part is composed as follows:
Aluminium dihydrogen phosphate-biphosphate chromium solution 1 ~ 4 part
Thinner 15 ~ 20 parts
Ceramic composition 20 ~ 40 parts.
Described aluminium dihydrogen phosphate-biphosphate chromium solution is made up of the raw material of following weight part:
The preparation method of described aluminium dihydrogen phosphate-biphosphate chromium solution is as follows:
The phosphoric acid solution that massfraction is 85% is taken according to ratio of quality and the number of copies, aluminium hydroxide, potassium bichromate or chromium trioxide, mixing and stirring obtains mixing solutions, mixing solutions is warming up to 120 DEG C ~ 150 DEG C and keeps 1h ~ 4h, temperature rise rate is 15 DEG C/min ~ 30 DEG C/min, 15 DEG C ~ 25 DEG C are cooled to after having reacted, the hydrogen peroxide or the formaldehyde that drip formula ratio wherein also fully stir, 15 DEG C ~ 25 DEG C are cooled to after being added dropwise to complete, then the acetone or alcohol adding formula ratio stirs, and obtains aluminium dihydrogen phosphate-biphosphate chromium mixing solutions.
Described thinner is made up of the raw material of following weight part:
Massfraction is the phosphoric acid solution 80 ~ 120 parts of 85%
Distilled water 50 ~ 80 parts.
The preparation method of described thinner is as follows:
Take according to ratio of quality and the number of copies the phosphoric acid solution that massfraction is 85%, distilled water, mixing and stirring, obtains thinner.
Described ceramic composition is made up of the raw material of following weight part:
Wherein, the particle size range of aluminum oxide is 20 μm ~ 200 μm; The particle size range of aluminium nitride is 200nm ~ 1000nm; The particle size range of silica powder is 5 μm ~ 50 μm; The particle size range of lithium Feldspar Powder is 5 μm ~ 50 μm; Zirconic particle size range is 300nm ~ 1000nm.
Wherein the particle diameter of aluminum oxide, aluminium nitride, silica powder, zirconium white, lithium Feldspar Powder all requires in particle size range, and particle diameter is crossed conference and caused coating material uneven; Calcium oxide, magnesium oxide specification of quality is in span of control, and quality too much can cause shorten working life; Tri-lead tetroxide, sodium tetraborate, tripoly phosphate sodium STPP specification of quality are in span of control, and quality too much can cause resistance to elevated temperatures to be deteriorated.
The preparation method of described ceramic composition is as follows:
Take aluminum oxide, aluminium nitride, zirconium white, silica powder, lithium Feldspar Powder, calcium oxide, magnesium oxide, tri-lead tetroxide, sodium tetraborate and tripoly phosphate sodium STPP by proportioning, with V-type mixer mixing 6h, obtain ceramic composition.
The concrete steps of the preparation method of phosphoric acid salt doped ceramics coating material of the present invention are as follows:
(1) take aluminium dihydrogen phosphate-biphosphate chromium solution by proportioning, thinner, mixing and stirring, after add the ceramic composition of proportional quantity, be mixed into even muddy, obtain phosphoric acid salt doped ceramics coating material;
(2) the phosphoric acid salt doped ceramics coated materials that step (1) obtains maybe can be glued material surface in metallic substance, control temperature is according to 50 DEG C ~ 150 DEG C, gradient increased temperature, time range is 12h ~ 48h, makes phosphoric acid salt doped ceramics hardened material shaping.
In step (2), gradient increased temperature requires that gradient temperature scope is no more than 30 DEG C.The too fast meeting that heats up causes material internal hole to increase, and the heating-up time will according to intensification requirement, and the heating-up time, the short hardened material that will cause not exclusively lost efficacy.
Positively effect of the present invention is as follows:
The present invention with alumina-zirconia-silica powder ceramic powder for matrix, the zirconium white wherein added has stronger wear resisting property, aluminium nitride, calcium oxide, magnesium oxide can improve the hardened forming speed of aluminium dihydrogen phosphate-biphosphate chromium solution, reduce the mold temperature of material, other powder can the pH value of regulation system, and play the effect of sintering aid, silica powder and lithium feldspar add the cost that can reduce material, in addition aluminium dihydrogen phosphate-biphosphate chromium solution and aluminum oxide, aluminium nitride is inorganic sizing agent component, for phosphoric acid salt doped ceramics material provides good adhesiveproperties, and pottery itself is high temperature resistant, corrosion resistance is stronger, therefore the phosphoric acid salt doped ceramics material prepared has wear-resisting, corrosion-resistant, high temperature resistant, the features such as cementability is strong.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1:
One, the phosphatase 11 00g, the potassium bichromate 2g that take massfraction 85% add in 500mL there-necked flask, mixing solutions are warming up to 50 DEG C, and stir 30min, until potassium bichromate dissolves formation orange solution completely with the speed of 500 ~ 800r/min; Orange solution is warming up to 70 DEG C, takes 20g aluminium hydroxide and be divided into 10 parts, add 1 part every 10min and constantly stir, all add rear continuation and stir 30min, dissolve completely to aluminium hydroxide; Then by solution warms to 140 DEG C, continue reaction 1.5h and constantly stir, being cooled to room temperature after completion of the reaction; Take 10g hydrogen peroxide more dropwise add wherein and constantly stir, after dropwising, be cooled to room temperature; Add 10mL acetone soln again to stir, obtained aluminium dihydrogen phosphate-biphosphate chromium solution;
Two, take phosphoric acid solution 100g and the distilled water 70g of massfraction 85%, by phosphoric acid solution and distilled water mixing and stirring, obtain thinner;
Three, aluminum oxide 15g is taken, zirconium white 12.5g, silica powder 10g, aluminium nitride 0.5g, calcium oxide 0.5g, magnesium oxide 0.25g, tri-lead tetroxide 1g, sodium tetraborate 0.4g, powder is dropped into V-type mixer mixing 6h by tripoly phosphate sodium STPP 0.4g, lithium feldspar 5g, obtains ceramic composition;
Four, take the aluminium dihydrogen phosphate that obtains in one, two, three-biphosphate chromium solution 4g, thinner 16g, ceramic composition 20g is mixed into even muddy, obtain phosphoric acid salt doped ceramics coating material.
The working life of phosphoric acid salt doped ceramics coating material: 30min ~ 120min.
The curing condition of phosphoric acid salt doped ceramics material: phosphoric acid salt doped ceramics coated materials maybe can be glued material surface surface in metallic substance, 50 DEG C of heating 4h, 70 DEG C of heating 4h, 90 DEG C of heating 8h, 130 DEG C of heating 4h, 150 DEG C of heating 6h, can make phosphoric acid salt doped ceramics hardened material.
The phosphoric acid salt doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, its surface is applied to the power of 50N, and material monolithic keeps complete and surperficial nothing is subsided.Be warming up to 1000 DEG C and test the thermal weight loss situation of phosphoric acid salt doped ceramics material, result thermal weight loss rate is 6.5%; Bonding 45# steel testing plate, according to " GB/T 7124-2008, the mensuration (rigid material is to rigid material) of sizing agent tensile shear strength ", normal temperature shearing resistance is 3.07MPa, and after 500 DEG C of process 1h, shearing resistance is 1.76MPa; Use stainless steel and phosphoric acid salt doped ceramics material to mill according to " the natural ornamental stone test method of GB/T 9966.4-2001 ", apply 25N pressure, rotating speed is 50rpm/min, and wear loss is 0.26g/cm
2.
Embodiment 2:
One, the phosphatase 11 00g, the potassium bichromate 2g that take massfraction 85% add in 500mL there-necked flask, mixing solutions are warming up to 50 DEG C, and stir 30min, until potassium bichromate dissolves formation orange solution completely with the speed of 500 ~ 800r/min; Orange solution is warming up to 70 DEG C, takes 20g aluminium hydroxide and be divided into 10 parts, add 1 part every 10min and constantly stir, all add rear continuation and stir 30min, dissolve completely to aluminium hydroxide; Then by solution warms to 140 DEG C, continue reaction 1.5h and constantly stir, being cooled to room temperature after completion of the reaction; Take 10g hydrogen peroxide more dropwise add wherein and constantly stir, after dropwising, be cooled to room temperature; Add 10mL acetone soln again to stir, obtained aluminium dihydrogen phosphate-biphosphate chromium solution;
Two, take phosphoric acid solution 100g and the distilled water 70g of massfraction 85%, by phosphoric acid solution and distilled water mixing and stirring, obtain thinner;
Three, take aluminum oxide 15g, zirconium white 12.5g, silica powder 10g, aluminium nitride 1g, calcium oxide 1g, magnesium oxide 0.5g, tri-lead tetroxide 1g, sodium tetraborate 0.4g, tripoly phosphate sodium STPP 0.4g, powder is dropped into V-type mixer mixing 6h by lithium feldspar 5g, obtains ceramic composition;
Four, take the aluminium dihydrogen phosphate that obtains in one, two, three-biphosphate chromium solution 4g, thinner 16g, ceramic composition 20g is mixed into even muddy, obtain phosphoric acid salt doped ceramics coating material.
The working life of phosphoric acid salt doped ceramics coating material: 20min ~ 60min.
The curing condition of phosphoric acid salt doped ceramics material: phosphoric acid salt doped ceramics coated materials maybe can be glued material surface surface in metallic substance, 50 DEG C of heating 3h, 70 DEG C of heating 3h, 90 DEG C of heating 6h, 130 DEG C of heating 3h, 150 DEG C of heating 6h, can make phosphoric acid salt doped ceramics hardened material.
The phosphoric acid salt doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, its surface is applied to the power of 50N, and material monolithic keeps complete and surperficial nothing is subsided.Be warming up to 1000 DEG C and test the thermal weight loss situation of phosphoric acid salt doped ceramics material, result thermal weight loss rate is 8.0%; Bonding 45# steel testing plate, according to " GB/T 7124-2008, the mensuration (rigid material is to rigid material) of sizing agent tensile shear strength ", normal temperature shearing resistance is 2.54MPa, and after 500 DEG C of process 1h, shearing resistance is 1.41MPa; Use stainless steel and phosphoric acid salt doped ceramics material to mill according to " the natural ornamental stone test method of GB/T 9966.4-2001 ", apply 25N pressure, rotating speed is 50rpm/min, and wear loss is 0.32g/cm
2.
Embodiment 3:
One, the phosphatase 11 00g, the potassium bichromate 2g that take massfraction 85% add in 500mL there-necked flask, mixing solutions are warming up to 50 DEG C, and stir 30min, until potassium bichromate dissolves formation orange solution completely with the speed of 500 ~ 800r/min; Orange solution is warming up to 70 DEG C, takes 20g aluminium hydroxide and be divided into 10 parts, add 1 part every 10min and constantly stir, all add rear continuation and stir 30min, dissolve completely to aluminium hydroxide; Then by solution warms to 140 DEG C, continue reaction 1.5h and constantly stir, being cooled to room temperature after completion of the reaction; Take 10g hydrogen peroxide more dropwise add wherein and constantly stir, after dropwising, be cooled to room temperature; Add 10mL acetone soln again to stir, obtained aluminium dihydrogen phosphate-biphosphate chromium solution;
Two, take phosphoric acid solution 100g and the distilled water 70g of massfraction 85%, by phosphoric acid solution and distilled water mixing and stirring, obtain thinner;
Three, aluminum oxide 15g is taken, zirconium white 12.5g, silica powder 10g, aluminium nitride 0.5g, calcium oxide 0.5g, magnesium oxide 0.25g, tri-lead tetroxide 1g, sodium tetraborate 0.4g, powder is dropped into V-type mixer mixing 6h by tripoly phosphate sodium STPP 0.4g, lithium feldspar 5g, obtains ceramic composition;
Four, take the aluminium dihydrogen phosphate that obtains in one, two, three-biphosphate chromium solution 4g, thinner 16g, ceramic composition 30g is mixed into even muddy, obtain phosphoric acid salt doped ceramics coating material.
The working life of phosphoric acid salt doped ceramics coating material: 30min ~ 120min.
The curing condition of phosphoric acid salt doped ceramics material: phosphoric acid salt doped ceramics coated materials maybe can be glued material surface surface in metallic substance, 50 DEG C of heating 4h, 70 DEG C of heating 4h, 90 DEG C of heating 8h, 130 DEG C of heating 4h, 150 DEG C of heating 6h, can make phosphoric acid salt doped ceramics hardened material.
The phosphoric acid salt doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, its surface is applied to the power of 50N, and material monolithic keeps complete and surperficial nothing is subsided.Be warming up to 1000 DEG C and test the thermal weight loss situation of phosphoric acid salt doped ceramics material, result thermal weight loss rate is 5.4%; Bonding 45# steel testing plate, according to " GB/T 7124-2008, the mensuration (rigid material is to rigid material) of sizing agent tensile shear strength ", normal temperature shearing resistance is 3.43MPa, and after 500 DEG C of process 1h, shearing resistance is 2.06MPa; Use stainless steel and phosphoric acid salt doped ceramics material to mill according to " the natural ornamental stone test method of GB/T 9966.4-2001 ", apply 25N pressure, rotating speed is 50rpm/min, and wear loss is 0.17g/cm
2.
Embodiment 4:
One, the phosphatase 11 00g, the potassium bichromate 2g that take massfraction 85% add in 500mL there-necked flask, mixing solutions are warming up to 50 DEG C, and stir 30min, until potassium bichromate dissolves formation orange solution completely with the speed of 500 ~ 800r/min; Orange solution is warming up to 70 DEG C, takes 20g aluminium hydroxide and be divided into 10 parts, add 1 part every 10min and constantly stir, all add rear continuation and stir 30min, dissolve completely to aluminium hydroxide; Then by solution warms to 140 DEG C, continue reaction 1.5h and constantly stir, being cooled to room temperature after completion of the reaction; Take 10g hydrogen peroxide more dropwise add wherein and constantly stir, after dropwising, be cooled to room temperature; Add 10mL acetone soln again to stir, obtained aluminium dihydrogen phosphate-biphosphate chromium solution;
Two, take phosphoric acid solution 100g and the distilled water 70g of massfraction 85%, by phosphoric acid solution and distilled water mixing and stirring, obtain thinner;
Three, aluminum oxide 15g is taken, zirconium white 12.5g, silica powder 10g, aluminium nitride 0.5g, calcium oxide 0.5g, magnesium oxide 0.25g, tri-lead tetroxide 1g, sodium tetraborate 0.4g, powder is dropped into V-type mixer mixing 6h by tripoly phosphate sodium STPP 0.4g, lithium feldspar 5g, obtains ceramic composition;
Four, take the aluminium dihydrogen phosphate that obtains in one, two, three-biphosphate chromium solution 8g, thinner 12g, ceramic composition 20g is mixed into even muddy, obtain phosphoric acid salt doped ceramics coating material.
The working life of phosphoric acid salt doped ceramics coating material: 30min ~ 90min.
The curing condition of phosphoric acid salt doped ceramics material: phosphoric acid salt doped ceramics coated materials maybe can be glued material surface surface in metallic substance, 50 DEG C of heating 6h, 70 DEG C of heating 6h, 90 DEG C of heating 12h, 130 DEG C of heating 6h, 150 DEG C of heating 8h, can make phosphoric acid salt doped ceramics hardened material.
The phosphoric acid salt doped ceramics material prepared according to above-mentioned technique, is warming up to 1200 DEG C, its surface is applied to the power of 50N, and material monolithic keeps complete and surperficial nothing is subsided.Be warming up to 1000 DEG C and test the thermal weight loss situation of phosphoric acid salt doped ceramics material, result thermal weight loss rate is 5.7%; Bonding 45# steel testing plate, according to " GB/T 7124-2008, the mensuration (rigid material is to rigid material) of sizing agent tensile shear strength ", normal temperature shearing resistance is 3.50MPa, and after 500 DEG C of process 1h, shearing resistance is 2.14MPa; Use stainless steel and phosphoric acid salt doped ceramics material to mill according to " the natural ornamental stone test method of GB/T 9966.4-2001 ", apply 25N pressure, rotating speed is 50rpm/min, and wear loss is 0.29g/cm
2.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (10)
1. a phosphoric acid salt doped ceramics coating material, is characterized in that: described phosphoric acid salt doped ceramics coating material is made up of aluminium dihydrogen phosphate-biphosphate chromium solution, thinner and ceramic composition, and its concrete weight part is composed as follows:
Aluminium dihydrogen phosphate-biphosphate chromium solution 1 ~ 4 part
Thinner 15 ~ 20 parts
Ceramic composition 20 ~ 40 parts.
2. phosphoric acid salt doped ceramics coating material as claimed in claim 1, is characterized in that: described aluminium dihydrogen phosphate-biphosphate chromium solution is made up of the raw material of following weight part:
3. phosphoric acid salt doped ceramics coating material as claimed in claim 2, is characterized in that: the preparation method of described aluminium dihydrogen phosphate-biphosphate chromium solution is as follows:
The phosphoric acid solution that massfraction is 85% is taken according to ratio of quality and the number of copies, aluminium hydroxide, potassium bichromate or chromium trioxide, mixing and stirring obtains mixing solutions, mixing solutions is warming up to 120 DEG C ~ 150 DEG C and keeps 1h ~ 4h, temperature rise rate is 15 DEG C/min ~ 30 DEG C/min, 15 DEG C ~ 25 DEG C are cooled to after having reacted, the hydrogen peroxide or the formaldehyde that drip formula ratio wherein also fully stir, 15 DEG C ~ 25 DEG C are cooled to after being added dropwise to complete, then the acetone or alcohol adding formula ratio stirs, and obtains aluminium dihydrogen phosphate-biphosphate chromium mixing solutions.
4. phosphoric acid salt doped ceramics coating material as claimed in claim 1, is characterized in that: described thinner is made up of the raw material of following weight part:
Massfraction is the phosphoric acid solution 80 ~ 120 parts of 85%
Distilled water 50 ~ 80 parts.
5. phosphoric acid salt doped ceramics coating material as claimed in claim 4, is characterized in that: the preparation method of described thinner is as follows:
Take according to ratio of quality and the number of copies the phosphoric acid solution that massfraction is 85%, distilled water, mixing and stirring, obtains thinner.
6. phosphoric acid salt doped ceramics coating material as claimed in claim 1, is characterized in that: described ceramic composition is made up of the raw material of following weight part:
7. phosphoric acid salt doped ceramics coating material as claimed in claim 6, is characterized in that: the particle size range of aluminum oxide is 20 μm ~ 200 μm; The particle size range of aluminium nitride is 200nm ~ 1000nm; The particle size range of silica powder is 5 μm ~ 50 μm; The particle size range of lithium Feldspar Powder is 5 μm ~ 50 μm; Zirconic particle size range is 300nm ~ 1000nm.
8. phosphoric acid salt doped ceramics coating material as claimed in claim 7, is characterized in that: the preparation method of described ceramic composition is as follows:
Take aluminum oxide, aluminium nitride, zirconium white, silica powder, lithium Feldspar Powder, calcium oxide, magnesium oxide, tri-lead tetroxide, sodium tetraborate and tripoly phosphate sodium STPP by proportioning, with V-type mixer mixing 6h, obtain ceramic composition.
9. prepare a method for the phosphoric acid salt doped ceramics coating material as described in any one of claim 1-8, it is characterized in that: the concrete steps of described preparation method are as follows:
(1) take aluminium dihydrogen phosphate-biphosphate chromium solution by proportioning, thinner, mixing and stirring, after add the ceramic composition of proportional quantity, be mixed into even muddy, obtain phosphoric acid salt doped ceramics coating material;
(2) the phosphoric acid salt doped ceramics coated materials that step (1) obtains maybe can be glued material surface in metallic substance, control temperature is according to 50 DEG C ~ 150 DEG C, gradient increased temperature, time range is 12h ~ 48h, makes phosphoric acid salt doped ceramics hardened material shaping.
10. preparation method as claimed in claim 9, is characterized in that: in step (2), and gradient increased temperature requires that gradient temperature scope is no more than 30 DEG C.
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| CN106336692A (en) * | 2015-11-17 | 2017-01-18 | 中国科学院兰州化学物理研究所 | Fastener coating, and preparation method and application thereof |
| CN109233564A (en) * | 2018-08-10 | 2019-01-18 | 南京世界村汽车动力有限公司 | A kind of locomotive engine high-temperature anticorrosion paint and preparation method thereof |
| CN116283321A (en) * | 2023-05-18 | 2023-06-23 | 中南大学 | Ablation-resistant coated zirconium-based phosphate material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106336692A (en) * | 2015-11-17 | 2017-01-18 | 中国科学院兰州化学物理研究所 | Fastener coating, and preparation method and application thereof |
| CN106336692B (en) * | 2015-11-17 | 2018-10-02 | 中国科学院兰州化学物理研究所 | A kind of fastener coating and its preparation method and application |
| CN109233564A (en) * | 2018-08-10 | 2019-01-18 | 南京世界村汽车动力有限公司 | A kind of locomotive engine high-temperature anticorrosion paint and preparation method thereof |
| CN116283321A (en) * | 2023-05-18 | 2023-06-23 | 中南大学 | Ablation-resistant coated zirconium-based phosphate material and preparation method thereof |
| CN116283321B (en) * | 2023-05-18 | 2023-08-11 | 中南大学 | Ablation-resistant coated zirconium-based phosphate material and preparation method thereof |
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