CN103818956B - The preparation technology of water quenching synthesizing flaky nano zirconia - Google Patents
The preparation technology of water quenching synthesizing flaky nano zirconia Download PDFInfo
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- CN103818956B CN103818956B CN201410097881.3A CN201410097881A CN103818956B CN 103818956 B CN103818956 B CN 103818956B CN 201410097881 A CN201410097881 A CN 201410097881A CN 103818956 B CN103818956 B CN 103818956B
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- water quenching
- powder
- preparation technology
- zirconia
- water
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- 238000010791 quenching Methods 0.000 title claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 230000000171 quenching effect Effects 0.000 title claims abstract description 31
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000010987 cubic zirconia Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Abstract
The present invention provides a kind of preparation technology of water quenching synthesizing flaky nano zirconia, belongs to technical field of nanometer material preparation.It is characterized in that：Using water quenching, with zirconium boride powder as raw material, powder granularity is 2~50 μm, and purity is more than 99%, 900~1100 DEG C of 0.2~1 h of insulation are heated to, water quenching, water quenching solution temperature is 10~30 DEG C, dried after water quenching, repeat operation 0~2 time above, obtain final product flake nano Zirconium powder.Present invention process is simple, and safe operation, low cost is not polluted, the flake nano zirconium oxide of synthesis, and 3 times of its thickness, and good dispersion are more than along the size of aspect parallel direction.
Description
Technical field
The present invention provides a kind of preparation technology of water quenching synthesizing flaky nano zirconia, belongs to nano material preparation technology
Field.
Background technology
Zirconium dioxide is a kind of high temperature resistant, wear-resistant, corrosion resistant Inorganic Non-metallic Materials, except being applied to traditional fire proofed wood
Outside material and ceramic paint, it is also widely used in high-tech areas such as electronic ceramics, function ceramics and structural ceramics.Nanometer
Structural material, such as nano wire, nanometer rods, nanometer sheet, show new physical property, have potential application in many fields.From
At present both at home and abroad to nanoscale ZrO2Research from the point of view of, the nanometer ZrO of preparation2Particle is mainly spherical and bar-shaped.At present on piece
Shape nano zircite preparation method has following technology to report：1st, the patent CN1008997B " lifes of flaky zirconia type fine crystals
Product method " prepares the flaky zirconia fine crystals of sulphate-containing ion using acidic aqueous solution, then at 110~350 DEG C
At a temperature of hydro-thermal process prepare four directions or cubic zirconia, 700 DEG C of calcinings are still four directions or cubic zirconia, and its sheet is thin
The thickness 7nm of grain crystal, the size along aspect parallel direction is about 100nm.Have the disadvantage that the hydrothermal synthesis reaction cycle is long, high temperature is high
Pressure, operational hazards are unfavorable for industrialized production；The size for generating crystal parallel direction is small；Reaction is carried out in sulfuric acid solution,
High cost, operational hazards are polluted to environment.2nd, " the preparation side of synthesizing sheeted zirconia by using hydrothermal of patent 2009100193840
With zirconium oxychloride and sodium borohydride as raw material, aqueous sodium carbonate is reaction medium to method ", and 5~120h is incubated at 120~300 DEG C
Prepare flaky zirconia.Have the disadvantage that the hydrothermal synthesis reaction cycle is long, HTHP, operational hazards, by autoclave volume
Limitation, combined coefficient is low, is unfavorable for industrialized production；Contain a large amount of sodium carbonate in generation product, reduce powder purity, need
Further to wash.
The content of the invention
Can overcome big drawbacks described above, fine crystals width, process is simple, operation peace it is an object of the invention to provide one kind
Entirely, low cost, the preparation technology of water quenching synthesizing flaky nano zirconia not polluted, its technical scheme is：
A kind of preparation technology of water quenching synthesizing flaky nano zirconia, it is characterised in that：Using water quenching, with zirconium boride
Powder is raw material, and powder granularity is 2~50 μm, and purity is more than 99 %, is heated to 900~1100 DEG C of 0.2~1 h of insulation, water quenching,
Water quenching solution temperature is 10~30 DEG C, is dried after water quenching, repeats operation 0~2 time above, obtains final product flake nano Zirconium powder.
The present invention compared with prior art, has the following advantages that：
1st, the present invention uses water quenching, compared with hydrothermal synthesis method, without using high-temperature high-pressure apparatus, operation peace
Entirely, efficiency high, is conducive to industrialized production；
2nd, the present invention is water quenching, does not use strong acid and strong base, and safe operation is not polluted to environment；
3rd, the flake nano zirconium oxide of present invention synthesis, 3 times of its thickness, and dispersion are more than along the size of aspect parallel direction
Property is good.
Brief description of the drawings
Fig. 1 is the XRD spectrums of powder after the present invention 1000 DEG C of calcinings, 10 DEG C of water quenchings；
Fig. 2 is the SEM photograph of powder after the present invention 1000 DEG C of calcinings, 10 DEG C of water quenchings.
Specific embodiment
Embodiment 1
With zirconium boride powder as raw material, powder granularity is 2 μm, and purity is more than 99 %, is heated to 1000 DEG C of 0.2 h of insulation,
Water quenching, water quenching solution temperature is 10 DEG C, is dried after water quenching, obtains final product flake nano Zirconium powder.
Tested by XRD, it is seen that powder crystal type is monoclinic phase（See Fig. 1）；Tested by SEM, it is seen that zirconia powder
Body is sheet, thick 150nm or so, a width of 500 nm or so（See Fig. 2）.
Embodiment 2
With zirconium boride powder as raw material, powder granularity is 20 μm, and purity is more than 99 %, is heated to 900 DEG C of 0.5 h of insulation,
Water quenching, water quenching solution temperature is 20 DEG C, is dried after water quenching, is repeated 1 times, and obtains final product flake nano Zirconium powder.
Embodiment 3
With zirconium boride powder as raw material, powder granularity is 50 μm, and purity is more than 99 %, is heated to 1100 DEG C of 1 h of insulation, water
Quench, water quenching solution temperature is 30 DEG C, dried after water quenching, be repeated 2 times, obtain final product flake nano Zirconium powder.
Claims (1)
1. a kind of preparation technology of water quenching synthesizing flaky nano zirconia, it is characterised in that：Using water quenching, with boronation zirconium powder
Body is raw material, and powder granularity is 2~50 μm, and purity is more than 99 %, is heated to 900~1100 DEG C of 0.2~1 h of insulation, water quenching, water
Solution temperature of quenching is 10~30 DEG C, is dried after water quenching, repeats operation 0~2 time above, obtains final product flake nano Zirconium powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410097881.3A CN103818956B (en) | 2014-03-17 | 2014-03-17 | The preparation technology of water quenching synthesizing flaky nano zirconia |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410097881.3A CN103818956B (en) | 2014-03-17 | 2014-03-17 | The preparation technology of water quenching synthesizing flaky nano zirconia |
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| Publication Number | Publication Date |
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| CN103818956A CN103818956A (en) | 2014-05-28 |
| CN103818956B true CN103818956B (en) | 2017-06-20 |
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| CN201410097881.3A Expired - Fee Related CN103818956B (en) | 2014-03-17 | 2014-03-17 | The preparation technology of water quenching synthesizing flaky nano zirconia |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386745B (en) * | 2014-11-03 | 2015-12-30 | 安徽工业大学 | A kind of preparation method of nano zirconium oxide powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3749763A (en) * | 1971-08-03 | 1973-07-31 | Humphreys Corp | Processing of silicate ores and product thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5978928A (en) * | 1982-10-25 | 1984-05-08 | Agency Of Ind Science & Technol | Manufacture of zirconia powder |
| JPH0233652B2 (en) * | 1986-03-11 | 1990-07-30 | Nippon Shokubai Kagaku Kogyo Kk | JIRUKONIAGANJUBIFUNMATSUNOSEIZOHOHO |
| CN101851005B (en) * | 2010-05-17 | 2011-08-31 | 山东理工大学 | Preparation method of high-dispersion zirconium oxide nano powder |
-
2014
- 2014-03-17 CN CN201410097881.3A patent/CN103818956B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3749763A (en) * | 1971-08-03 | 1973-07-31 | Humphreys Corp | Processing of silicate ores and product thereof |
Non-Patent Citations (3)
| Title |
|---|
| 制备条件对ZrO2晶型的影响-四方ZrO2生成条件考察;韦薇;《天然气化工》;19991231;第24卷;第7-11页 * |
| 化学沉淀法制备纳米氧化锆的研究;王焕英等;《河北师范大学学报(自然科学版)》;20020930;第26卷(第5期);第488-491页 * |
| 纳米氧化锆粉体的制备;范增为等;《陶瓷》;20071231(第4期);第29-32页 * |
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