CN103588211A - Preparation method of spherical zirconium silicate nano aggregate powder - Google Patents
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Abstract
The invention relates to a preparation method of spherical zirconium silicate nano aggregate powder, and belongs to the technical field of an inorganic material. The preparation method comprises the steps as follows: zirconium oxychloride and sodium metasilicate are mixed with water, precipitation is separated out, and washing and drying are performed to obtain a precursor; sodium fluoride and water are added into the precursor and reacts at the temperature of 180-380 DEG C for 4-10 hours to obtain zirconium silicate powder containing impurities; the zirconium silicate powder containing impurities is mixed with water and filtered and washed by an inorganic membrane separation device to obtain concentrated slurry, pie powder is obtained through pressure filtration, and zirconium silicate powder is obtained through drying; the zirconium silicate powder and absolute ethyl alcohol are mixed, and ground and emulsified in a colloid mill so as to obtain a mixed turbid liquid of the zirconium silicate nano powder and absolute ethyl alcohol; and the mixed turbid liquid is processed by a liquid powder feeder and inductive plasma spheroidization equipment, the zirconium silicate nano powder of the mixed turbid liquid is subjected to agglomeration, spheroidization and densification process to obtain the powder. The method is simple and low in cost, the spherical zirconium silicate nano aggregate powder can be directly prepared, and the purity quality is improved.
Description
Technical field
The present invention relates to a kind of zirconium silicate (ZrSiO
4) preparation method of ball shaped nano coacervate powder, belong to technical field of inorganic material.
Background technology
Along with the development of Aeronautics and Astronautics technology, the use temperature of aircraft engine hot-end component and body, pressure require to improve constantly.Correspondingly, high temperature resistant, the antioxidant property for aircraft engine hot-end component and material that body is used had higher requirement.Zirconium silicate (ZrSiO
4) be a kind of silicate compound with tetragonal system island structure, zirconium white with YSZ(stabilized with yttrium oxide) compare, there is higher specific refractory power, more excellent high-temperature-phase structural stability, chemical stability (as acid-alkali-corrosive-resisting), fabulous thermal shock resistance and antioxidant property preferably, based on described advantage, make zirconium silicate material extensive in aerospace field application prospect.Ball shaped nano reunion powder can for thermospray, sintering and etc. static pressure etc. using the moulding process of powder body material as raw material.
At present, the method for preparing the original nano-powder of zirconium silicate mainly contains the several different methods such as solid phase method, the precipitator method, hydrothermal method, sol-gel method.In the preparation process of coacervate powder, the original nano-powder of zirconium silicate generally need to pass through the techniques such as calcining, mist projection granulating and high temperature sintering, after the above-mentioned art breading of process, the original nano-powder crystal grain overwhelming majority is often grown up for micron crystal grain, making the coacervate powder finally making is micron order, under in nodulizing, between a plurality of nano-powder small-particles, can stick together and become a micron spherical powder; Using zirconium silicate micron coacervate powder during as raw material, in the coating structure being made by it, have hardly nanostructure, be difficult to represent nano coating performance advantage; Meanwhile, the spherical powder surface of micron is generally relatively more loose, coarse, and bonding strength is lower, affects its use properties; And the subsequent disposal operation of prior art too much, too numerous and diverse.In view of this, in the urgent need to developing a kind of preparation method of new zirconium silicate nanoclusters aggressiveness powder, overcome above shortcoming.
Summary of the invention
For the nanocrystal existing in prior art, be difficult to the shortcoming retaining, the spherical powder surface of micron exists more defect, the object of the invention is to provide a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, described method is by the adjustment to related process parameter, can obtain the surface compact of certain particle size range distribution, bright and clean, solid ball shaped nano coacervate powder, described powder has excellent flowing property, high-temperature-phase Stability Analysis of Structures, chemical stability are better, in heat barrier coat material field, have good application prospect.
The object of the invention is to be achieved through the following technical solutions.
A preparation method for zirconium silicate ball shaped nano coacervate powder, described method steps is as follows:
(1) basic zirconium chloride and Starso are mixed with water as raw material, isolate precipitation and wash, dry, obtain presoma; Wherein, the mol ratio of basic zirconium chloride and Starso is 0.8～1.5:1, and the mass ratio of water and raw material is 6～10:1;
(2) in presoma, add mineralizer Sodium Fluoride (NaF) and water to carry out hydro-thermal reaction, temperature of reaction is 180 ℃～380 ℃, and the reaction times is 4h～10h, obtains impure zirconium silicate powder; Wherein, the mol ratio of fluorine element and zr element is 2:1;
(3) impure zirconium silicate powder step (2) being obtained mixes with water, adopt mineral membrane isolation technique to filter and wash, obtain concentrated slurry, will concentrate slurry press filtration and obtain pie powder, dry, obtain zirconium silicate powder, wherein, mineral membrane isolation technique adopts inorganic diaphragm separator to carry out, working pressure is 0.15MPa～0.25MPa, wash temperature is 50 ℃～80 ℃, and the dehydration rate of concentrated slurry is 50%～70%, and the pH value of concentrated slurry is 6～8;
(4) zirconium silicate powder step (3) being obtained mixes with dehydrated alcohol, puts into that colloidal mill grinds, emulsification, obtains the suspension liquid that mixes of zirconium silicate nanometer powder body and dehydrated alcohol;
(5) zirconium silicate nanometer powder body step (4) being obtained and dehydrated alcohol mix the liquid powder feeder of suspension liquid utilization and induction plasma nodularization equipment is processed, to the zirconium silicate nanometer powder body in described suspension liquid reunite, nodularization and densification, obtain described a kind of zirconium silicate ball shaped nano coacervate powder;
Wherein, the water in step (1), (2) and (3) is water more than purity >=deionized water purity.
In step (3), the film that the separated preferably use of mineral membrane aperture is 50nm～2 μ m, working pressure is 0.2MPa, the pH value of concentrated slurry is 7; Press filtration can adopt pressure filter to carry out, and preferably the disposable material mouth through pressure filter of concentrated slurry adds it interior to 2/3 of pressure filter volume, and pressure filter internal pressure is 0.5Kg/cm
2; It is dry that pie powder can be placed in baking oven, and 5h～24h preferably dewaters at 100 ℃.
In step (4), preferably the mass ratio of zirconium silicate powder and dehydrated alcohol is 1:5～8; Preferably the rotating speed of colloidal mill is 2880r/min, and the zirconium silicate nanometer powder body now obtaining has good mobility with dehydrated alcohol mixing suspension liquid.
In step (5), utilizing liquid powder feeder and induction plasma nodularization equipment to process can adopt method specific as follows: zirconium silicate nanometer powder body is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, and the particle after atomization, after induction plasma heating, nodularization, densification occurs; In treating processes, preferably plasma power is 28KW～30KW, atomizing gas flow is 5slpm～7slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm～7slpm, argon flow amount is 50slpm～60slpm, chamber pressure is 8psia～12psia, and powder feeder rotating speed is 6r/mim～8r/mim; The zirconium silicate ball shaped nano coacervate powder surface obtaining is bright and clean, fine and close, and size distribution is 20 μ m～100 μ m.
Beneficial effect
1, the invention provides a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, described method can directly prepare zirconium silicate ball shaped nano coacervate powder from the original nano-powder of zirconium silicate, not only can avoid the introducing of impurity, meanwhile, the purity of powder is improved; Described method is simple, has reduced the preparation cost of zirconium silicate ball shaped nano coacervate powder;
2. the invention provides a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, described method is utilized the advantage that hydrothermal method synthesis reaction temperature is lower on the one hand, can effectively slow down the growth of zirconium silicate crystal grain, effectively avoid zirconium silicate powder generation hard aggregation, make zirconium silicate particles keep nanocrystalline structure; On the other hand, compare with calcining process with atomizing granulating technology, by using liquid powder feeding technology and induction plasma spheronization techniques to prepare fine and close zirconium silicate ball shaped nano coacervate powder, prevent the generation of defect, effectively stop the introducing of impurity, guaranteed purity and the quality of product;
In described method steps (3), preferred film aperture is 50nm～2 μ m, pressure is 0.2MPa, there is higher detersive efficiency, the median size of the concentrated slurry mesosilicic acid zirconium powder body obtaining after washing and the distribution range of particle diameter are more conducive to subsequent disposal, and this is that traditional filtration and separating technology is incomparable;
3. the invention provides a kind of preparation method of zirconium silicate ball shaped nano coacervate powder, the size distribution that described method can make is the zirconium silicate ball shaped nano coacervate powder of 20 μ m～100 μ m, mobility can reach 30s～45s/50g, can meet preferably the requirement of plasma spraying, there is not grain growth and hard aggregation phenomenon simultaneously, the primary granule particle diameter of described powder, below 100nm, maintains nanostructure in the coating that it is prepared.
Accompanying drawing explanation
Fig. 1 is the transmission electron micrograph of the zirconium silicate ball shaped nano coacervate powder primary granule for preparing of embodiment 1.
Fig. 2 is the scanning electron microscope diagram sheet of the zirconium silicate ball shaped nano coacervate powder for preparing of embodiment 1.
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of implementing the 1 zirconium silicate ball shaped nano coacervate powder preparing.
Embodiment
Below by embodiment, the invention will be further described, but embodiment does not limit the scope of the invention.
The zirconium silicate ball shaped nano coacervate powder that following examples are prepared is tested as follows:
(1) morphology observation:
Adopt NEC JEM-2100 type transmission electron microscope to observe and pattern and the size of measuring the primary granule of described powder; Adopt the pattern of coacervate powder described in the Japanese new and high technology S-4800 of Co., Ltd. type awkward silence at a meeting emission scan electron microscope observation;
(2) X-ray diffraction analysis:
X ' the Pert PRO MPD type polycrystal X ray diffraction analysis instrument that adopts Dutch PANalytical company to produce is analyzed; Test conditions: Cu target, K α, Ni filter plate; Tube voltage 40kV, tube current 40mA; Slit sizes DS=0.957 °, PSD=2.12,4 °/min of sweep velocity;
(3) mobility-detected:
The FL4-1 type device for measuring flowability that utilizes Iron and Steel Research Geueral Inst to produce detects; Testing method: the needed time of standard funnel that crosses predetermined hole diameter with flow of powder described in 50g represents.
(1) by 31.70g eight water basic zirconium chloride (ZrOCl
28H
2o), 34.97g non-hydrate sodium metasilicate (Na
2siO
39H
2o) as raw material, mix with 500g deionized water, isolate precipitation through deionized water wash, 100 ℃ of oven dryings, the powder obtaining is presoma;
(2) in 18g presoma, add 8.26g mineralizer Sodium Fluoride (NaF) to mix with 1L deionized water, insert in 1.5L cartridge type reactor and carry out hydro-thermal reaction, the reaction times is 4h, and temperature of reaction is 180 ℃, obtain impure zirconium silicate powder, now powder occurs soft-agglomerated;
(3) the impure zirconium silicate powder of the 18g obtaining in step (2) is mixed with 4L deionized water, adopt inorganic diaphragm separator to wash, filter and obtain concentrated slurry, wherein the working pressure of inorganic diaphragm separator is 0.2MPa～0.25MPa, wash temperature is 70 ℃～80 ℃, membrane pore size is 100nm, the dehydration rate of concentrated slurry is 50%～70%, and the pH value of the concentrated slurry obtaining through mineral membrane separating treatment is 7; Concentrated slurry adopts pressure filter to carry out press filtration processing, and the disposable material mouth through pressure filter of concentrated slurry adds it interior to volume 2/3, and pressure filter internal pressure is 0.5Kg/cm
2, obtain pie powder, dry through 100 ℃, baking oven, obtain zirconium silicate powder;
(4) 100g zirconium silicate powder being mixed with 500g dehydrated alcohol, put in colloidal mill, is grinding, emulsification under 2880r/min condition at rotating speed, obtains zirconium silicate nanometer powder body and dehydrated alcohol mixing suspension liquid;
(5) zirconium silicate nanometer powder body obtaining in step (4) is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, after induction plasma heating, there is nodularization in the particle after atomization, densification, the parameter of induction plasma nodularization equipment is: plasma power is 28KW, the flow of atomizing gas argon gas is 5slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm, argon flow amount is 50slpm, chamber pressure is 8psia, powder feeder rotating speed is 6r/mim, obtain a kind of zirconium silicate ball shaped nano coacervate powder of the present invention.
The zirconium silicate ball shaped nano coacervate powder that the present embodiment is prepared detects, and result is as follows:
(1) morphology microstructure:
The pattern of described powder as illustrated in fig. 1 and 2, as shown in Figure 1, obtains the floccule mass aggressiveness that a plurality of particle accumulations to piece are, and each nano particle is of a size of 10nm～25nm; As shown in Figure 2, described coacervate powder is surface compact and smooth spherical, and size distribution is 20 μ m～70 μ m;
(2) X-ray diffraction analysis:
The X ray diffracting spectrum of described powder as shown in Figure 3, meets well with the X ray diffracting spectrum (JCPD, NO.80-1807) of standard zirconium silicate, and characteristic peak all occurs, and the appearance of assorted peak, illustrates and prepares the zirconium silicate powder that purity is higher;
(3) mobility-detected:
Known after testing, the flowing property of described powder is 36s/50g.
Embodiment 2
(1) 41.98g eight water basic zirconium chlorides, 24.69g non-hydrate sodium metasilicate are made into mixing solutions as raw material and 650g deionized water, isolate precipitation through deionized water wash, 100 ℃ of oven dryings, the powder obtaining is presoma.
(2) in 24g presoma, add 10.94g mineralizer Sodium Fluoride to mix with 1L deionized water, insert 1.5L cartridge type reactor and carry out hydro-thermal reaction, the reaction times is 10h, and temperature of reaction is 380 ℃, obtain impure zirconium silicate powder, now powder occurs soft-agglomerated;
(3) the impure zirconium silicate powder of the 24g obtaining in step (2) is mixed with 4L deionized water, adopt inorganic diaphragm separator to wash, filter and obtain concentrated slurry, wherein the working pressure of inorganic diaphragm separator is 0.2MPa～0.25MPa, wash temperature is 70 ℃～80 ℃, membrane pore size is 100nm, the dehydration rate of concentrated slurry is 50%～70%, and the pH value of the concentrated slurry obtaining through mineral membrane separating treatment is 7; Concentrated slurry carries out press filtration processing through pressure filter, and the disposable material mouth through pressure filter of concentrated slurry adds it interior to volume 2/3, and pressure filter internal pressure is 0.5Kg/cm
2, obtain pie powder, dry through 100 ℃, baking oven, obtain zirconium silicate powder;
(4) 100g zirconium silicate powder being mixed with 800g dehydrated alcohol, put in colloidal mill, is grinding, emulsification under 2880r/min condition at rotating speed, obtains zirconium silicate nanometer powder body and dehydrated alcohol mixing suspension liquid;
(5) zirconium silicate nanometer powder body obtaining in step (4) is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, after induction plasma heating, there is nodularization in the particle after atomization, densification, the parameter of induction plasma nodularization equipment is: plasma power is 30KW, the flow of atomizing gas argon gas is 7slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm, argon flow amount is 60slpm, chamber pressure is 12psia, powder feeder rotating speed is 8r/mim, obtain a kind of zirconium silicate ball shaped nano coacervate powder of the present invention.
The zirconium silicate ball shaped nano coacervate powder that the present embodiment is prepared detects, and result is as follows:
(1) morphology microstructure:
The floccule mass aggressiveness that obtains a plurality of particle accumulations to piece, each nano particle is of a size of 5nm～50nm; Described coacervate powder is surface compact and smooth spherical, and size distribution is 20 μ m～80 μ m;
(2) X-ray diffraction analysis:
The X ray diffracting spectrum (JCPD, NO.80-1807) of the X ray diffracting spectrum of described powder and standard zirconium silicate meets well, and characteristic peak all occurs, and the appearance of assorted peak, illustrates and prepares the zirconium silicate powder that purity is higher;
(3) mobility-detected:
Known after testing, the flowing property of described powder is 40s/50g.
Embodiment 3
(1) by 35.42g eight water basic zirconium chlorides, 31.25g non-hydrate sodium metasilicate mixes with 500g deionized water as raw material, isolates precipitation through deionized water wash, 100 ℃ of oven dryings, and the powder obtaining is presoma;
(2) in 20g presoma, add 9.22g mineralizer Sodium Fluoride to mix with 1L deionized water, insert 1.5L cartridge type reactor and carry out hydro-thermal reaction, the reaction times is 6h, and temperature of reaction is 200 ℃, obtains impure zirconium silicate powder, and now powder occurs soft-agglomerated;
(3) the impure zirconium silicate powder of the 20g obtaining in step (2) is mixed with 4L deionized water, adopt inorganic diaphragm separator to wash, filter and obtain concentrated slurry, wherein the working pressure of inorganic diaphragm separator is 0.2MPa～0.25MPa, wash temperature is 70 ℃～80 ℃, membrane pore size is 100nm, concentrated slurry dehydration rate be 50%～70%, the pH value of the concentrated slurry obtaining through mineral membrane separating treatment is 7; Concentrated slurry carries out press filtration processing through pressure filter, and the disposable material mouth through pressure filter of concentrated slurry adds it interior to volume 2/3, and pressure filter internal pressure is 0.5Kg/cm
2, obtain pie powder, dry through 100 ℃, baking oven, obtain zirconium silicate powder;
(4) 100g zirconium silicate powder being mixed with 600g dehydrated alcohol, put in colloidal mill, is grinding, emulsification under 2880r/min condition at rotating speed, obtains zirconium silicate nanometer powder body and dehydrated alcohol mixing suspension liquid;
(5) zirconium silicate nanometer powder body obtaining in step (4) is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, after induction plasma heating, there is nodularization in the particle after atomization, densification, the parameter of induction plasma nodularization equipment is: plasma power is 29KW, the flow of atomizing gas argon gas is 6slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 7slpm, argon flow amount is 50slpm, chamber pressure is 11psia, powder feeder rotating speed is 7r/mim, obtain a kind of zirconium silicate ball shaped nano coacervate powder of the present invention.
The zirconium silicate ball shaped nano coacervate powder that the present embodiment is prepared detects, and result is as follows:
(1) morphology microstructure:
The floccule mass aggressiveness that obtains a plurality of particle accumulations to piece, each nano particle is of a size of 10nm～40nm; Described coacervate powder is surface compact and smooth spherical, and size distribution is 30 μ m～100 μ m;
(2) X-ray diffraction analysis:
The X ray diffracting spectrum (JCPD, NO.80-1807) of the X ray diffracting spectrum of described powder and standard zirconium silicate meets well, and characteristic peak all occurs, and the appearance of assorted peak, illustrates and prepares the zirconium silicate powder that purity is higher;
(3) mobility-detected:
Known after testing, the flowing property of described powder is 48s/50g.
Claims (8)
1. a preparation method for zirconium silicate ball shaped nano coacervate powder, is characterized in that: step is as follows:
(1) basic zirconium chloride and Starso are mixed with water as raw material, isolate precipitation and wash, dry, obtain presoma; The mol ratio of basic zirconium chloride and Starso is 0.8～1.5:1, and the mass ratio of water and raw material is 6～10:1;
(2) in presoma, add Sodium Fluoride and water to carry out hydro-thermal reaction, temperature of reaction is 180 ℃～380 ℃, and the reaction times is 4h～10h, obtains impure zirconium silicate powder; The mol ratio of fluorine element and zr element is 2:1;
(3) impure zirconium silicate powder is mixed with water, with inorganic diaphragm separator, filter and wash, obtain concentrated slurry, will concentrate slurry press filtration and obtain pie powder, dry, obtain zirconium silicate powder; The working pressure of inorganic diaphragm separator is 0.15MPa～0.25MPa, and wash temperature is 50 ℃～80 ℃, and the dehydration rate of concentrated slurry is 50%～70%, and the pH value of concentrated slurry is 6～8;
(4) zirconium silicate powder is mixed with dehydrated alcohol, put into that colloidal mill grinds, emulsification, obtain the suspension liquid that mixes of zirconium silicate nanometer powder body and dehydrated alcohol;
(5) zirconium silicate nanometer powder body is processed with liquid powder feeder and induction plasma nodularization equipment with the suspension liquid that mixes of dehydrated alcohol, to the zirconium silicate nanometer powder body in described suspension liquid reunite, nodularization and densification, obtain described a kind of zirconium silicate ball shaped nano coacervate powder;
Water in step (1), (2) and (3) is water more than purity >=deionized water purity.
2. the preparation method of a kind of zirconium silicate ball shaped nano coacervate powder according to claim 1, is characterized in that: inorganic diaphragm separator is used the film that aperture is 50nm～2 μ m, and working pressure is 0.2MPa, and the pH value of concentrated slurry is 7.
3. the preparation method of a kind of zirconium silicate ball shaped nano coacervate powder according to claim 1 and 2, it is characterized in that: press filtration adopts pressure filter, the disposable material mouth through pressure filter of concentrated slurry adds it interior to 2/3 of volume, and pressure filter internal pressure is 0.5Kg/cm
2.
4. the preparation method of a kind of zirconium silicate ball shaped nano coacervate powder according to claim 1, is characterized in that: it is dry that pie powder is placed in baking oven, and 5h～24h dewaters at 100 ℃.
5. the preparation method of a kind of zirconium silicate ball shaped nano coacervate powder according to claim 1, is characterized in that: the mass ratio of zirconium silicate powder and dehydrated alcohol is 1:5～8.
6. a kind of preparation method of zirconium silicate ball shaped nano coacervate powder according to claim 1 or 5, is characterized in that: the rotating speed of colloidal mill is 2880r/min.
7. the preparation method of a kind of zirconium silicate ball shaped nano coacervate powder according to claim 1, it is characterized in that: utilize liquid powder feeder and induction plasma nodularization equipment to process, concrete steps are as follows: zirconium silicate nanometer powder body is sent into induction plasma spray gun body with the suspension liquid that mixes of dehydrated alcohol through liquid powder feeder, under atomizing gas ar gas acting, described suspension liquid is atomized, and the particle after atomization, after induction plasma heating, nodularization, densification occurs.
8. the preparation method of a kind of zirconium silicate ball shaped nano coacervate powder according to claim 7, it is characterized in that: treating processes applying plasma power is 28KW～30KW, atomizing gas flow is 5slpm～7slpm, the working gas of plasma body is the mixed gas of hydrogen and argon gas, hydrogen flowing quantity is 6slpm～7slpm, argon flow amount is 50slpm～60slpm, and chamber pressure is 8psia～12psia, and powder feeder rotating speed is 6r/mim～8r/mim.
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| CN103922354A (en) * | 2014-04-24 | 2014-07-16 | 北京化工大学 | High-yield zirconium silicate powder synthesized by sol-gel method |
| CN105110345A (en) * | 2015-08-03 | 2015-12-02 | 景德镇陶瓷学院 | Preparation method for Pr doped ZrSiO4 yellow ceramic pigment, product prepared thereby and application thereof |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN105236431A (en) * | 2015-08-28 | 2016-01-13 | 北京理工大学 | Preparation method of spherical nano zirconium silicate powder |
| CN105236431B (en) * | 2015-08-28 | 2017-05-10 | 北京理工大学 | Preparation method of spherical nano zirconium silicate powder |
| CN108483454A (en) * | 2017-08-16 | 2018-09-04 | 漳州市安泰锆业发展有限公司 | A kind of preparation process of carrier model nanoscale zirconium silicate |
| CN110938281A (en) * | 2019-12-13 | 2020-03-31 | 北京理工大学 | Modified carbon fiber reinforced phenolic resin matrix composite material and preparation thereof |
| CN113929474A (en) * | 2021-12-16 | 2022-01-14 | 矿冶科技集团有限公司 | Particulate matter for thermal barrier coating, preparation method of particulate matter, thermal barrier coating and engine |
| CN113929474B (en) * | 2021-12-16 | 2022-03-04 | 矿冶科技集团有限公司 | Particulate matter for thermal barrier coating, preparation method of particulate matter, thermal barrier coating and engine |
| CN115521070A (en) * | 2022-11-29 | 2022-12-27 | 广东大角鹿新材料有限公司 | Nano ultra-white overglaze, ceramic tile and preparation method thereof |
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