CN108483492A - A kind of preparation method of zirconia aerogels - Google Patents
A kind of preparation method of zirconia aerogels Download PDFInfo
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- CN108483492A CN108483492A CN201810345911.6A CN201810345911A CN108483492A CN 108483492 A CN108483492 A CN 108483492A CN 201810345911 A CN201810345911 A CN 201810345911A CN 108483492 A CN108483492 A CN 108483492A
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- zirconium
- zirconia aerogels
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000004964 aerogel Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011240 wet gel Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000352 supercritical drying Methods 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 8
- 238000006073 displacement reaction Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 235000019441 ethanol Nutrition 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000499 gel Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000002243 precursor Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 4
- 238000009413 insulation Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 3
- 238000003980 solgel method Methods 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 zirconium iso-propoxides Chemical class 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the preparation fields of new material, are related to a kind of preparation method of zirconia aerogels.This method is presoma, acid for catalyst using organic zirconates, inhibits the generation of precipitation by low temperature, quickly prepares zirconium oxide wet gel, zirconium oxide wet gel obtains blocky zirconia aerogels by solvent displacement and supercritical drying.Sol gel process of the present invention is simple, and prepared zirconia aerogels specific surface area is high, thermal conductivity is low, can be used for the fields such as heat-insulation and heat-preservation, catalyst and catalyst carrier.
Description
Technical field
The invention belongs to the preparation fields of new material, and in particular to a kind of preparation method of zirconia aerogels.
Background technology
As a kind of nano-porous materials, aeroge has three-D nano-porous network structure, assigns its low-density, high ratio
The characteristics such as surface area, macroporosity have the performances such as excellent heat-insulated, absorption, catalysis, in industrial production, building energy conservation, aviation
The fields such as space flight are widely used.Zirconia aerogels not only have the typical structure characteristic of aeroge, in heat-insulation and heat-preservation field
There is a good application prospect, but also with the conventional oxidations silicon airsetting such as the double property of soda acid, oxidisability and reproducibility, characteristic of semiconductor
Characteristic not available for glue makes the fields such as its catalysis except heat-insulation and heat-preservation, catalyst carrier, absorption all be widely used
Foreground.The preparation method of zirconia aerogels has the organic zirconates method of acid catalysis, propylene oxide induction inorganic zirconium salts method, the heating of alcohol water
Method etc..But current preparation method technique is more complex, or is unable to get blocky zirconia aerogels (such as precipitation method and alcohol water add
Hot method).Inhibit to precipitate caused by fast hydrolyzing-polymerization of zirconium oxide presoma by low temperature environment, passes through Fast sol-gel
Reaction obtains blocky zirconia aerogels.
Invention content
The purpose of the invention is to improve the deficiency of existing zirconia aerogels technology of preparing, and provide a kind of oxidation
The preparation method of zirconium aeroge.The zirconia aerogels preparation method is simple, quick, compensates for the preparation of conventional oxidation zirconium aeroge
Technologic deficiency.
The object of the invention technical solution is:A kind of preparation method of zirconia aerogels, is as follows:
At (1) -20~0 DEG C, deionized water is added after 1~10min is mixed in zirconium oxide presoma, solvent, acid, after
After 1~5min of continuous stirring, mixed liquor is placed in progress 5~30min of sol gel reaction at -10~10 DEG C and obtains wet gel,
Middle zirconium oxide presoma:Solvent:Deionized water:The molar ratio of acid is 1:(6~18):(2~4.5):(0.1~1);
(2) wet gel that step (1) obtains is subjected to solvent displacement at 0~20 DEG C with organic solvent;
(3) wet gel for obtaining step (2) carries out CO2Supercritical drying obtains zirconia aerogels.
Zirconium oxide presoma described in preferred steps (1) is one kind in zirconium-n-propylate, zirconium-n-butylate or zirconium iso-propoxide.
Solvent described in preferred steps (1) is one kind in ethyl alcohol, normal propyl alcohol, isopropanol or n-butanol.
Acid described in preferred steps (1) is one kind in nitric acid or hydrochloric acid.
Speed of agitator is 300-500 revs/min in preferred steps (1).
Organic solvent described in preferred steps (2) is one kind in ethyl alcohol, isopropanol or acetone.
Solvent time swap is 1~3 day in preferred steps (2), replaces an organic solvent within during which every 4~12 hours.
Advantageous effect:
(1) prepared by zirconia aerogels uses low-temperature sol-gel technique, can solve conventional preparation techniques and easy to produce
The shortcomings that precipitation.
(2) zirconia aerogels prepared by are that bulk material is answered compared with other zirconia aerogels nano particles
It is wider with range.
Description of the drawings
Fig. 1 is the pore size distribution curve of zirconia aerogels made from example 1.
Fig. 2 is the stereoscan photograph of zirconia aerogels made from example 1.
Specific implementation mode
Example 1
At 0 DEG C, by 0.1mol zirconium-n-propylates, 1.2mol ethyl alcohol, 0.1mol nitric acid be mixed 1min (rotating speed be 300 turns/
Minute) 0.2mol deionized waters are added afterwards, continue to stir after 5min (rotating speed be 300 revs/min) by mixed liquor be placed at 0 DEG C into
Row sol gel reaction 30min obtains wet gel, and wet gel carries out solvent displacement at 0 DEG C with ethyl alcohol, and (period every 12 is small within 3 days
Ethyl alcohol of Shi Genghuan) CO is carried out afterwards2Supercritical drying obtains zirconia aerogels.Zirconia aerogels density 0.115g/cm3,
Specific surface area 353m2/ g, Hotdisk thermal conductivity 0.026W/ (mK).
Referring to attached drawing, Fig. 1 is the pore size distribution curve of zirconia aerogels made from example 1.Pore-size distribution test uses
Merck & Co., Inc of U.S. ASAP2020 type hole structural analysis instrument.Pore size distribution curve shows the network of synthesized zirconia aerogels
Structure has typical aerogel pore structure feature based on mesoporous.
Referring to attached drawing, Fig. 2 is the stereoscan photograph of zirconia aerogels made from example 1.Sem test uses
Zeiss 1530VP scanning electron microscope.As can be seen that the net of the zirconia aerogels prepared by the present invention from SEM photograph
Network structure has aerogel material typical structural characteristics based on mesoporous.
Example 2
At -5 DEG C, by (rotating speed after 0.1mol zirconium-n-butylates, 1.8mol n-butanols, 0.01mol nitric acid mixing 10min
It is 400 revs/min) 0.3mol deionized waters are added, continue to be placed in mixed liquor after stirring 1min (rotating speed is 400 revs/min)
Sol gel reaction 5min is carried out at 10 DEG C and obtains wet gel, and wet gel carries out solvent with acetone at 20 DEG C and replaces 1 day (phase
Between every 4 hours replace an acetone) carry out CO afterwards2Supercritical drying obtains zirconia aerogels.Zirconia aerogels density
0.101g/cm3, specific surface area 410m2/ g, Hotdisk thermal conductivity 0.025W/ (mK).
Example 3
At -20 DEG C, by (rotating speed after 0.1mol zirconium iso-propoxides, 1.0mol isopropanols, 0.02mol mixed in hydrochloric acid stirring 8min
It is 300 revs/min) 0.25mol deionized waters are added, continue to be placed in mixed liquor after stirring 5min (rotating speed is 300 revs/min)
Sol gel reaction 10min is carried out at 5 DEG C and obtains wet gel, and wet gel carries out solvent with isopropanol at 0 DEG C and replaces 3 day (phase
Between replace an isopropanol for every eight hours) carry out CO afterwards2Supercritical drying obtains zirconia aerogels.Zirconia aerogels density
0.118g/cm3, specific surface area 350m2/ g, Hotdisk thermal conductivity 0.026W/ (mK).
Example 4
At -15 DEG C, by (rotating speed after 0.1mol zirconium-n-propylates, 0.6mol normal propyl alcohols, 0.06mol mixed in hydrochloric acid stirring 4min
It is 500 revs/min) 0.45mol deionized waters are added, continue to set mixed liquor after stirring 3min (rotating speed is 500 revs/min)
Sol gel reaction 20min is carried out at -10 DEG C and obtains wet gel, and wet gel carries out solvent with acetone at 10 DEG C and replaces 2 days
(every 10 hours of period replaced an acetone) carries out CO afterwards2Supercritical drying obtains zirconia aerogels.Zirconia aerogels are close
Spend 0.121g/cm3, specific surface area 219m2/ g, Hotdisk thermal conductivity 0.028W/ (mK).
Example 5
At -10 DEG C, 0.1mol zirconium-n-propylates, 1.4mol ethyl alcohol, 0.08mol nitric acid is mixed after 2min to (rotating speed is
300 revs/min) 0.4mol deionized waters are added, continue that mixed liquor is placed in -5 after stirring 1min (rotating speed is 300 revs/min)
Sol gel reaction 15min is carried out at DEG C and obtains wet gel, and wet gel carries out solvent with ethyl alcohol at 20 DEG C and replaces 1 day (period
Replace an ethyl alcohol within every 6 hours) CO is carried out afterwards2Supercritical drying obtains zirconia aerogels.Zirconia aerogels density
0.109g/cm3, specific surface area 347m2/ g, Hotdisk thermal conductivity 0.025W/ (mK).
Claims (7)
1. a kind of preparation method of zirconia aerogels, is as follows:
At (1) -20~0 DEG C, deionized water is added after 1~10min is mixed in zirconium oxide presoma, solvent, acid, continues to stir
After mixing 1~5min, mixed liquor is placed in progress 5~30min of sol gel reaction at -10~10 DEG C and obtains wet gel, wherein oxygen
Change zirconium precursor body:Solvent:Deionized water:The molar ratio of acid is 1:(6~18):(2~4.5):(0.1~1);
(2) wet gel that step (1) obtains is subjected to solvent displacement at 0~20 DEG C with organic solvent;
(3) wet gel for obtaining step (2) carries out CO2Supercritical drying obtains zirconia aerogels.
2. preparation method according to claim 1, it is characterised in that the zirconium oxide presoma described in step (1) is positive third
One kind in alcohol zirconium, zirconium-n-butylate or zirconium iso-propoxide.
3. preparation method according to claim 1, it is characterised in that solvent described in step (1) be ethyl alcohol, normal propyl alcohol,
One kind in isopropanol or n-butanol.
4. preparation method according to claim 1, it is characterised in that the acid described in step (1) is in nitric acid or hydrochloric acid
It is a kind of.
5. preparation method according to claim 1, it is characterised in that speed of agitator is 300-500 revs/min in step (1)
Clock.
6. preparation method according to claim 1, it is characterised in that organic solvent described in step (2) is ethyl alcohol, different
One kind in propyl alcohol or acetone.
7. preparation method according to claim 1, it is characterised in that solvent time swap is 1~3 day in step (2), the phase
Between every 4~12 hours replace an organic solvent.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108997010A (en) * | 2018-10-06 | 2018-12-14 | 景德镇陶瓷大学 | A kind of zero-emission oxide ceramic powder body preparation method and its production system |
CN111617301A (en) * | 2020-06-24 | 2020-09-04 | 深圳市天麒检测技术服务有限公司 | Simulation plant for removing mold in humid indoor air |
CN112562944A (en) * | 2020-12-11 | 2021-03-26 | 国网黑龙江省电力有限公司电力科学研究院 | Selective coating method suitable for hardware surface coating in strong wind and sand area |
Citations (2)
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CN103011280A (en) * | 2012-11-27 | 2013-04-03 | 天津大学 | Preparation method of zirconium oxide aerogel |
CN103523829A (en) * | 2013-10-08 | 2014-01-22 | 同济大学 | Preparation method of lumpy zirconia aerogel having high specific surface area |
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2018
- 2018-04-18 CN CN201810345911.6A patent/CN108483492A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103011280A (en) * | 2012-11-27 | 2013-04-03 | 天津大学 | Preparation method of zirconium oxide aerogel |
CN103523829A (en) * | 2013-10-08 | 2014-01-22 | 同济大学 | Preparation method of lumpy zirconia aerogel having high specific surface area |
Non-Patent Citations (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108997010A (en) * | 2018-10-06 | 2018-12-14 | 景德镇陶瓷大学 | A kind of zero-emission oxide ceramic powder body preparation method and its production system |
CN111617301A (en) * | 2020-06-24 | 2020-09-04 | 深圳市天麒检测技术服务有限公司 | Simulation plant for removing mold in humid indoor air |
CN112562944A (en) * | 2020-12-11 | 2021-03-26 | 国网黑龙江省电力有限公司电力科学研究院 | Selective coating method suitable for hardware surface coating in strong wind and sand area |
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