CN102649576B - Preparation process for flaky alumina with great diameter-thickness ratio - Google Patents
Preparation process for flaky alumina with great diameter-thickness ratio Download PDFInfo
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- CN102649576B CN102649576B CN 201210154460 CN201210154460A CN102649576B CN 102649576 B CN102649576 B CN 102649576B CN 201210154460 CN201210154460 CN 201210154460 CN 201210154460 A CN201210154460 A CN 201210154460A CN 102649576 B CN102649576 B CN 102649576B
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- tabular alumina
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- aluminum oxide
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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 large 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 larger 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 characteristics that the tabular alumina fusing point is high, hardness greatly, also has higher physical strength and easily disperse, 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].Research is found, the fracture toughness property of the ceramic matric composite that the ceramic matric composite that strengthens with tabular alumina strengthens with particulate alumina is high, 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, it is micron order on the radial dimension, thereby the dual nature that has had both nano-powder and micro-powder, embody good sticking power and moderate surfactivity, can with the effective combination of other active 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 the fields such as pearly pigment, makeup, automobile finish, filler and abrasive material [process engineering journal, 2004,4(supplementary issue): 279-283, coatings industry, 2004,34(1): 59-63].
The main method of preparation tabular alumina also is molten-salt growth method, and the people such as Yang Ying [process engineering journal, 2004,4(supplementary issue): 279-283] take Tai-Ace S 150 as raw material, complex vitriolate (Na
2SO
4+ K
2SO
4) be fused salt, be aided with outer doping (such as phosphoric acid salt, titanium dioxide or silicon-dioxide etc.), having synthesized thickness is the tabular alumina of 200-400nm.The people such as Zhang Qianying [the investigation of materials journal, 2008,22(2): 205-208] also take Tai-Ace S 150 as raw material, with the Al (OH) of sol-gel method preparation
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 impact 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 the reunion between the minimizing powder and staggered growth, the reunion of acquisition nothing and favorable dispersity) the aluminum oxide wafer, add TiOSO
4After, 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, without the sheet α that reunites-Al
2O
3The people such as Zhu [Ceramics International34 (2008) 1729 – 1733] are with Al (OH)
3Obtain the aluminum oxide of porous 500 ℃ of calcinings, take it as presoma, film-making shape aluminum oxide in NaCl – KCl fused salt, research finds 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.The people such as Lee [Materials Science and Engineering A 466 (2007) 79 – 83] take γ-Al2O3 as raw material, Na
2SO
4Be fused salt, studied the impact of microwave sintering on the tabular alumina pattern, research finds to adopt the tabular alumina size distribution of microwave sintering preparation even, but the radius-thickness ratio value is less.
Finding from above-mentioned research, is the tabular alumina that raw material can obtain larger radius-thickness ratio value with aluminium salt, but is that raw materials cost is higher with aluminium salt, is the tabular alumina that raw material then is difficult to obtain large radius-thickness ratio value with aluminum oxide.
Summary of the invention
The purpose of this invention is to provide a kind of take aluminum oxide as raw material, in raw material, add template, the shaping agent, but accelerating oxidation aluminium is grown to the sheet of rule, obtain large 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 large is characterized in that, comprises the steps:
(1) in aluminum oxide powder, adds template, fused salt and shaping agent, then mix, described template is a kind of in kaolin, graphite, calcite and the mica, add-on is the 0.01-5% of aluminum oxide powder quality, the add-on of described fused salt is the 100-300% of aluminum oxide powder quality, and the add-on of described shaping agent is the 0.01-5% of aluminum oxide powder quality;
(2) with the material that mixes behind reaction 1-4h under 800-1200 ℃ the temperature, obtain reaction product;
(3) with the water soaking 3-24h of reaction product with 40-100 ℃, after filtering, washing, be that 20-60 ℃, mass concentration are that the hydrofluoric acid solution of 10%-40% soaks 1-10h with temperature, obtain the large tabular alumina of radius-thickness ratio value after filtration, washing, the drying.
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 dioxide, zinc oxide, stannic oxide, ferric oxide and the silicon oxide.
Waste water after the usefulness hydrofluoric acid solution washing by soaking reaction product described in the step (3) is processed rear discharging with Wingdale, and the waste residue of generation is as the raw material of cement.
Advantage of the present invention is that take aluminum oxide as raw material, the material that adds sheet is template, can promote forming core and the growth of tabular alumina, obtains the tabular alumina (radius-thickness ratio is greater than 60) of large radius-thickness ratio.In raw material, add the shaping agent, but accelerating oxidation aluminium is grown to the hexagon of rule, makes simultaneously the particle diameter of flaky alumina even.
Description of drawings
Fig. 1 is the tabular alumina microstructure photo of the large radius-thickness ratio value prepared of the embodiment of the invention 6.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Table 1 has been listed 10 embodiment the first step processing condition that are numbered 1-10: kind and the add-on of determining template, fused salt, shaping agent according to the different embodiment of table 1.
The proportioning of table 1. raw material
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 determine sintering temperature and time according to table 2, obtain reaction product.And definite reaction product washing temperature and time, 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 |
As can be seen from Table 3, the tabular alumina radius-thickness ratio of the inventive method preparation value is controlled, alumina wafer smooth surface as can be seen from Figure 1, regular shape.
Claims (3)
1. the tabular alumina preparation technology that the radius-thickness ratio value is large is characterized in that, comprises the steps:
(1) in aluminum oxide powder, adds template, fused salt and shaping agent, then mix, described template is a kind of in kaolin, graphite, calcite and the mica, add-on is the 0.01-5% of aluminum oxide powder quality, the add-on of described fused salt is the 100-300% of aluminum oxide powder quality, and described shaping agent is a kind of in titanium dioxide, zinc oxide, the stannic oxide, and add-on is the 0.01-5% of aluminum oxide powder quality;
(2) with the material that mixes behind reaction 1-4h under 800-1200 ℃ the temperature, obtain reaction product;
(3) with the water soaking 3-24h of reaction product with 40-100 ℃, after filtering, washing, be that 20-60 ℃, mass concentration are that the hydrofluoric acid solution of 10%-40% soaks 1-10h with temperature, obtain the large tabular alumina of radius-thickness ratio value after filtration, washing, the drying.
2. the large tabular alumina preparation technology of radius-thickness ratio value as claimed in claim 1, 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 the sodium sulfate of 1:1 and sodium-chlor that vitriolate of tartar, mol ratio are 1:1 and the Repone K.
3. the large tabular alumina preparation technology of radius-thickness ratio value as claimed in claim 1, it is characterized in that, waste water after the usefulness hydrofluoric acid solution washing by soaking reaction product described in the step (3) is processed rear discharging with Wingdale, and the waste residue of generation is as the raw material of cement.
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| 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 |
| CN112225557B (en) * | 2020-10-16 | 2022-03-04 | 江西德锆美瓷有限公司 | Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method |
| CN112978775B (en) * | 2021-04-19 | 2023-07-25 | 陕西科技大学 | Method for preparing high-aspect ratio flaky alumina by taking lotus roots as templates |
| CN115259188B (en) * | 2022-08-02 | 2024-02-27 | 郑州大学 | Flaky alumina sandwich composite material and preparation method thereof |
Citations (1)
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|---|---|---|---|---|
| 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 |
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| 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 (4)
| Title |
|---|
| 片状氧化铝应用与制备研究;马小玲;《山东陶瓷》;20111231;第34卷(第6期);第18-21页 * |
| 用高岭土制备片状氧化铝粉体;谭宏斌等;《耐火材料》;20091231;第43卷(第6期);第453-455页 * |
| 谭宏斌等.用高岭土制备片状氧化铝粉体.《耐火材料》.2009,第43卷(第6期),第453-455页. |
| 马小玲.片状氧化铝应用与制备研究.《山东陶瓷》.2011,第34卷(第6期),第18-21页. |
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