CN102649576A - Preparation process for flaky alumina with great diameter-thickness ratio - Google Patents
Preparation process for flaky alumina with great diameter-thickness ratio Download PDFInfo
- Publication number
- CN102649576A CN102649576A CN2012101544600A CN201210154460A CN102649576A CN 102649576 A CN102649576 A CN 102649576A CN 2012101544600 A CN2012101544600 A CN 2012101544600A CN 201210154460 A CN201210154460 A CN 201210154460A CN 102649576 A CN102649576 A CN 102649576A
- Authority
- CN
- China
- Prior art keywords
- thickness ratio
- radius
- tabular alumina
- big
- ratio value
- 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.)
- Granted
Links
Images
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation process for flaky alumina with a great diameter-thickness ratio. The preparation process comprises the following steps of: adding fused salt in alumina powder; adding a template agent; adding a shaping agent and then uniformly mixing; filling a mixture into a crucible with a cover; after reacting at the set temperature, washing soluble salts with hot water; and dissolving an impurity phase in a hydrofluoric acid solution and washing and drying to obtain the flaky alumina. According to the method, the template agent and the shaping agent are added to obtain the regular flaky alumina with the great diameter-thickness ratio. The method has the characteristics of simple process and easiness for industrial production. The flaky alumina prepared by the invention can be used as a composite material enhanced phase, a high-grade abrasive, a substrate of pearl pigment and filler of a polymer material.
Description
Technical field
The present invention relates to the preparation method of the big tabular alumina of a kind of radius-thickness ratio value, the tabular alumina of preparation can be used as and is matrix material wild phase, the base material of senior abrasive, pearly pigment and the filler of macromolecular material.
Background technology
The tabular alumina crystal formation is α-A1
2O
3(corundum type) has bigger diameter (5-50 μ m) and less thickness (0.10-0.50 μ m), the α-A1 of perfect crystalline
2O
3Particle is the regular hexagonal shape.The tabular alumina fusing point is high, hardness greatly, also has higher physical strength and easy dispersive characteristics; Can be used as the wild phase of metal, pottery and glass based composite material; Improve Young's modulus, toughness and intensity [Journal of the European Ceramic Society 19 (1999) 335 – 339 of matrix material; Journal of the European Ceramic Society 25 (2005) 1541 – 1550, Ceramics International 30 (2004) 785 – 791].Discover; The fracture toughness property with particulate alumina enhanced ceramic matric composite is high with tabular alumina enhanced ceramic matric composite; Because tabular alumina produces the bridge joint effect in matrix, can improve the toughness [Journal of Physics and Chemistry of Solids 69 (2008) 1521 – 1524] of material.The thickness dimension of tabular alumina is nano level or is bordering on nano level; Be micron order on the radial dimension, thereby had both the dual nature of nano-powder and micro-powder, embody good sticking power and moderate surfactivity; Can effectively combine with other reactive group; Be difficult for again reuniting, powder itself is close to colourless, transparent, has the ability of significant shielding effect and reflection ray; Therefore, tabular alumina also can be used for fields [process engineering journal, 2004,4 (supplementary issue): 279-283, coatings industry, 2004,34 (1): 59-63] such as pearly pigment, makeup, automobile finish, filler and abrasive material.
The main method of preparation tabular alumina also is a molten-salt growth method, and people such as Yang Ying [process engineering journal, 2004,4 (supplementary issue): 279-283] are raw material with Tai-Ace S 150, complex vitriolate (Na
2SO
4+ K
2SO
4) be fused salt, be aided with outer doping (like phosphoric acid salt, titanium oxide or silicon-dioxide etc.), having synthesized thickness is the tabular alumina of 200-400nm.People such as Zhang Qianying [investigation of materials journal, 2008,22 (2): 205-208] also are raw material with Tai-Ace S 150, with the Al (OH) of Prepared by Sol Gel Method
3Precursor is at Na
2SO
4-K
2SO
4Synthetic α-A1 in the fused salt
2O
3Powder has been studied Na
3PO
412H
2O and TiOSO
4Additive is to α Al
2O
3The influence of pattern.Additive Na
3PO
412H
2But the phosphate anion among the O is stopped the growth of surface adsorption inhibited oxidation aluminium crystal on thickness direction at crystalline substance, and reunion between the minimizing powder and staggered growth, reunion of acquisition nothing and good dispersibility) the aluminum oxide wafer, add TiOSO
4After, the entering of titanium ion can improve the aluminium vacancy concentration, thereby changes the speed of growth of each crystal face of crystal, impels its comparatively formation of regular morphology, thereby prepare pattern rule, size evenly, do not have a sheet α-Al that reunites
2O
3People such as Zhu [Ceramics International34 (2008) 1729 – 1733] are with Al (OH)
3Obtaining the porous aluminum oxide 500 ℃ of calcinings, is presoma with it, and film-making shape aluminum oxide in NaCl – KCl fused salt discover that having obtained median size at 900 ℃ of calcining 4h is the tabular alumina of 2.4 μ m, but the radius-thickness ratio value is less.People such as Lee [Materials Science and Engineering A 466 (2007) 79 – 83] are raw material, Na with γ-Al2O3
2SO
4Be fused salt, studied the influence of microwave sintering, discover that the tabular alumina size distribution that adopts microwave sintering to prepare is even, but the radius-thickness ratio value is less the tabular alumina pattern.
Discover from above-mentioned, use aluminium salt can obtain the tabular alumina of big radius-thickness ratio value, but use aluminium salt higher, use aluminum oxide then to be difficult to obtain the tabular alumina of big radius-thickness ratio value as raw material as raw materials cost as raw material.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with the aluminum oxide; In raw material, add template, the shaping agent, but promotes oxidn aluminium is grown to the sheet of rule; Obtain big radius-thickness ratio value (the radius-thickness ratio value is greater than 60) tabular alumina preparation technology, can significantly reduce preparation cost.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
The tabular alumina preparation technology that a kind of radius-thickness ratio value is big is characterized in that, comprises the steps:
(1) in aluminum oxide powder, adds template; Fused salt and shaping agent; Mix then, said template is a kind of in kaolin, graphite, calcite and the mica, and add-on is the 0.01-5% of aluminum oxide powder quality; The add-on of said fused salt is the 100-300% of aluminum oxide powder quality, and the add-on of said shaping agent is the 0.01-5% of aluminum oxide powder quality;
(2) with the material that mixes under 800-1200 ℃ the temperature reaction 1-4h after, obtain reaction product;
(3) with the water logging bubble 3-24h of reaction product with 40-100 ℃; After filtering, washing; Use temperature to soak 1-10h as the hydrofluoric acid solution of 10%-40%, obtain the big tabular alumina of radius-thickness ratio value after filtration, washing, the drying as 20-60 ℃, mass concentration.
In the such scheme, the fused salt described in the step (1) is that sodium sulfate, vitriolate of tartar, sodium-chlor, sodium phosphate, sodium hydrogen phosphate, trisodium phosphate, Repone K, mol ratio are a kind of in 1: 1 sodium sulfate and vitriolate of tartar, the mol ratio sodium-chlor that is 1: 1 and the Repone K.
Shaping agent described in the step (1) is a kind of in titanium oxide, zinc oxide, White tin oxide, red stone and the silicon oxide.
Described in the step (3) with the waste water after the hydrofluoric acid solution washing by soaking reaction product, handle the back discharging with Wingdale, the waste residue of generation is as the raw material of cement.
Advantage of the present invention is, is raw material with the aluminum oxide, and adding flaky material is template, can promote the forming core and the growth of tabular alumina, obtains the tabular alumina (radius-thickness ratio is greater than 60) of big radius-thickness ratio.In raw material, add the shaping agent, but promotes oxidn aluminium is grown to the hexagon of rule, makes the particle diameter of flaky alumina even simultaneously.
Description of drawings
The tabular alumina microstructure photo of the big radius-thickness ratio value that Fig. 1 prepares for the embodiment of the invention 6.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed description.
Table 1 has been listed 10 embodiment the first step processing condition that are numbered 1-10: kind and the add-on of confirming template, fused salt, shaping agent according to table 1 various embodiment.
Table 1. proportion of raw materials
Table 2 has been listed second step, the three step process condition of table 1 embodiment: mixture is packed in the crucible with cover, and different embodiment confirm sintering temperature and time according to table 2, obtain reaction product.And definite reaction product washing temperature and time, the concentration and the time of pickling temperature, acid, obtain tabular alumina after the drying.
The preparation process condition of table 2 tabular alumina
The radius-thickness ratio value of embodiment of the invention tabular alumina is shown in table 3.
The radius-thickness ratio value of table 3 tabular alumina
| The embodiment numbering | The diameter of tabular alumina (μ m) | Tabular alumina maximum diameter thickness rate value |
| 1 | ?20 | 40 |
| 2 | ?30 | 45 |
| 3 | ?25 | 40 |
| 4 | ?35 | 45 |
| 5 | 40 | 43 |
| 6 | 30 | 60 |
| 7 | 28 | 48 |
| 8 | 36 | 48 |
| 9 | 38 | 46 |
| 10 | 28 | 42 |
Can find out that from table 3 the tabular alumina radius-thickness ratio value of the inventive method preparation is controlled, can find out alumina wafer smooth surface, regular shape from Fig. 1.
Claims (4)
1. the tabular alumina preparation technology that the radius-thickness ratio value is big is characterized in that, comprises the steps:
(1) in aluminum oxide powder, adds template; Fused salt and shaping agent; Mix then, said template is a kind of in kaolin, graphite, calcite and the mica, and add-on is the 0.01-5% of aluminum oxide powder quality; The add-on of said fused salt is the 100-300% of aluminum oxide powder quality, and the add-on of said shaping agent is the 0.01-5% of aluminum oxide powder quality;
(2) with the material that mixes under 800-1200 ℃ the temperature reaction 1-4h after, obtain reaction product;
(3) with the water logging bubble 3-24h of reaction product with 40-100 ℃; After filtering, washing; Use temperature to soak 1-10h as the hydrofluoric acid solution of 10%-40%, obtain the big tabular alumina of radius-thickness ratio value after filtration, washing, the drying as 20-60 ℃, mass concentration.
2. the tabular alumina preparation technology that radius-thickness ratio value as claimed in claim 1 is big; It is characterized in that the fused salt described in the step (1) is that sodium sulfate, vitriolate of tartar, sodium-chlor, sodium phosphate, sodium hydrogen phosphate, trisodium phosphate, Repone K, mol ratio are a kind of in 1: 1 sodium sulfate and vitriolate of tartar, the mol ratio sodium-chlor that is 1: 1 and the Repone K.
3. the tabular alumina preparation technology that radius-thickness ratio value as claimed in claim 1 is big is characterized in that, the shaping agent described in the step (1) is a kind of in titanium oxide, zinc oxide, White tin oxide, red stone and the silicon oxide.
4. the tabular alumina preparation technology that radius-thickness ratio value as claimed in claim 1 is big; It is characterized in that; Described in the step (3) with the waste water after the hydrofluoric acid solution washing by soaking reaction product, handle the back discharging with Wingdale, the waste residue of generation is as the raw material of cement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210154460 CN102649576B (en) | 2012-05-18 | 2012-05-18 | Preparation process for flaky alumina with great diameter-thickness ratio |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210154460 CN102649576B (en) | 2012-05-18 | 2012-05-18 | Preparation process for flaky alumina with great diameter-thickness ratio |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102649576A true CN102649576A (en) | 2012-08-29 |
| CN102649576B CN102649576B (en) | 2013-10-23 |
Family
ID=46691708
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210154460 Expired - Fee Related CN102649576B (en) | 2012-05-18 | 2012-05-18 | Preparation process for flaky alumina with great diameter-thickness ratio |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102649576B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087676A (en) * | 2013-01-29 | 2013-05-08 | 淄博理研泰山涂附磨具有限公司 | Sintering method of abrasion resisting abrasive particles |
| CN112225557A (en) * | 2020-10-16 | 2021-01-15 | 江西德锆美瓷有限公司 | Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method |
| CN112978775A (en) * | 2021-04-19 | 2021-06-18 | 陕西科技大学 | Method for preparing flake alumina with high aspect ratio by taking lotus roots as template |
| CN115259188A (en) * | 2022-08-02 | 2022-11-01 | 郑州大学 | Flaky alumina sandwich composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775659B (en) * | 2010-01-14 | 2011-11-23 | 陕西理工学院 | Process for preparing mullite whisker or flaky alumina by using coal ash |
-
2012
- 2012-05-18 CN CN 201210154460 patent/CN102649576B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775659B (en) * | 2010-01-14 | 2011-11-23 | 陕西理工学院 | Process for preparing mullite whisker or flaky alumina by using coal ash |
Non-Patent Citations (2)
| Title |
|---|
| 谭宏斌等: "用高岭土制备片状氧化铝粉体", 《耐火材料》, vol. 43, no. 6, 31 December 2009 (2009-12-31), pages 453 - 455 * |
| 马小玲: "片状氧化铝应用与制备研究", 《山东陶瓷》, vol. 34, no. 6, 31 December 2011 (2011-12-31), pages 18 - 21 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087676A (en) * | 2013-01-29 | 2013-05-08 | 淄博理研泰山涂附磨具有限公司 | Sintering method of abrasion resisting abrasive particles |
| CN103087676B (en) * | 2013-01-29 | 2014-07-30 | 淄博理研泰山涂附磨具有限公司 | Sintering method of abrasion resisting abrasive particles |
| CN112225557A (en) * | 2020-10-16 | 2021-01-15 | 江西德锆美瓷有限公司 | Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method |
| CN112978775A (en) * | 2021-04-19 | 2021-06-18 | 陕西科技大学 | Method for preparing flake alumina with high aspect ratio by taking lotus roots as template |
| CN115259188A (en) * | 2022-08-02 | 2022-11-01 | 郑州大学 | Flaky alumina sandwich composite material and preparation method thereof |
| CN115259188B (en) * | 2022-08-02 | 2024-02-27 | 郑州大学 | Flaky alumina sandwich composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102649576B (en) | 2013-10-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101775659B (en) | Process for preparing mullite whisker or flaky alumina by using coal ash | |
| CN105645933B (en) | A kind of laminated structure Ceramic corundum abrasive and preparation method thereof | |
| CN102649576B (en) | Preparation process for flaky alumina with great diameter-thickness ratio | |
| KR101823170B1 (en) | Composite inorganic particles and methods of making and using the same | |
| JPH10504348A (en) | Modified sol-gel alumina | |
| CN104370300A (en) | High-dispersity spherical cerium oxide powder and preparation method thereof | |
| CN110678432B (en) | Composition for completely or partially replacing ball clay in ceramic and preparation method and application thereof | |
| EP3121150B1 (en) | Plate-like aluminum oxide and preparation method therefor | |
| CN101597078B (en) | Method for preparing flake alpha-Al2O3 granular powder | |
| CN104402029B (en) | A kind of high dispersive α-Al 2o 3the preparation method of nanometer sheet | |
| CN107326432B (en) | A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics | |
| JP6254913B2 (en) | Method for producing α-lithium aluminate | |
| CN104891541B (en) | The method that aluminium carbonate ammonium pyrolysismethod prepares flaky alumina | |
| JP5538399B2 (en) | Corundum crystal structure pigments with low soluble chromium content | |
| CN107777715B (en) | A kind of high dispersive slab-like Alpha-alumina micro mist and preparation method thereof | |
| CN101337808B (en) | Process for preparing alpha-alumina powder for ceramic film support | |
| CN104692442A (en) | Method for preparing high-purity and high-strength gypsum through medium- and low-level phosphorite associated calcium sources | |
| CN103570005A (en) | Soluble salt assisted mechanical ball-milling method for preparing graphene nano sheet powder | |
| KR101440473B1 (en) | Method for preparing plate-shaped alumina | |
| CN107311223B (en) | A kind of sheet magnesium titanate potassium and preparation method thereof | |
| CN110228963A (en) | A kind of novel artificial quartzite plate | |
| CN108367932B (en) | Beta-zeolite and process for producing the same | |
| Sarfraz et al. | Synthesis and characterization of nano hydroxyapatite | |
| Gao et al. | The application of nanoparticle ceramic materials in the design of modern handicrafts | |
| CN106115707A (en) | A kind of antioxidative crystalline flake graphite powder body and preparation method thereof |
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: 20131023 Termination date: 20170518 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |