• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Alpha-alumina consisting essentially of solid, spherical, non-aggregated particles, having a diameter from 0.06 to 2 µm, a polydispersion index not greater than 2.0. a total porosity less than 0.3 cc/g, a specific surface area from 0.7 to 80 m2/lg, and an apparent density of the particles from 3.2 to 3.94 g/cm3. Such alpha-alumina is prepared by a process wherein an alpha-alumina precursor, having a water content from 2 to 35% by weight, at starting temperatures from room temperature to 850°C, having a particle diameter from 0.07 to 2.3 µm and a polydispersion index not greater than 2.0, is subjected to a heat-treatment at temperatures ranging from 1130° to 1700°C, the precursor being instantaneously brought from the starting temperature to the treatment temperature, and by carrying out the treatment during times. generally indicated in Figure 1 between straight lines (a) and (b), which are sufficient to convert the precursor to the alpha phase, but not such as to cause disgregation and/or aggregation; the resulting product being then brought again to room temperature by means of a non-instantaneous cooling of the order of at least 10 seconds.
    公开号:SU1709901A3
    申请号:SU864013919
    申请日:1986-01-15
    公开日:1992-01-30
    发明作者:Мелло Череза Эмильяно；Дженнаро Антонио；Кортези Паоло
    申请人:Монтэдисон С.П.А. (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for producing spherical non-aggregated particles (yi-alumina used as an electronic material in the manufacture of substrates (junction conductors or packaging for integrated circuits, as ceramic materials, especially in the manufacture of turbine blades, pipes for sodium lamps or as catalysts or catalyst supports for heterogeneous canalization
    A known method for producing spherical od-alumina, which includes the heat treatment of hydrated alumina and the subsequent cooling of the resulting product, However
    The resulting product cannot be used to make ceramics.
    The purpose of the invention is the expansion of technological capabilities by using a product for the manufacture of ceramics.
    The proposed (X-oxide. Aluminum is a solid spherical non-aggregated particles, the average linear diameter of which is I 0.06 - 2 microns, polydispersity index
    -: - less than or equal to 2.0 (where
    权利要求:
    Claims (3)
    [1]
    the weighted average diameter, a, is the average linear diameter), the total porosity of the micromestotype is below 0.3, the specificity 1 on the surface is 0.7 and 80, the density of particles is 3.2 - 3.9 g / cm. Microtip porosity of having a diameter of less than 20 A. Mesotype - the presence of pores having a diameter in the range from 20 to 500 Average sizes a and d, as well as morphological and granulometric characteristics are determined under an electron microscope in accordance with the translucent method In electron microscopy, products with an average diameter of 0.1-1 µm and a polydispersity index less than or equal to 1.30 are used predominantly, and if the diameters are in the range of 0.2-0.6 µm, then the product is monodisperse, i.e. polydispersity index is less than or equal to. The proposed (x Aluminum OXID has a very low porosity of the micromix type (less than 0.1) or even succeeds in obtaining non-porous 0-alumina. 0 -0-alumina can be obtained in a mixture with other crystalline phases, such as delta and / cly theta-alumina. These mixtures contain 70 masD or more cx-phases. Particles of different formed phases in the mixture are spherical non-aggregated and monodisperse or polydisperse. Purity-alumina - or a mixture comprising u i-alumina , until psd pkr 99, e8 masd, sometimes yes 99.99 wt / 4. The proposed process for the preparation of o-alumina or its mixture with delta and / or theta alumina consists in the heat treatment of the starting compound containing hydrated alumina, amorphous or crystalline, with a water content 2 to 35 May. Or -alumina or a mixture of. Indicated starting compounds in the form of spherical non-aggregated particles having a dispersion field index less than or equal to 2, an average linear diameter of 0.07 µm, by instantaneously increasing the temperature of the starting compound from temperatures in the range from room temperature to 850 ° C to temperatures of heat treatment in the range from 1130 to over a period of time sufficient for conversion. starting the compound to (y; - phase, but not long enough to aggregate and / or destroy the product, and then lowering the temperature of the resulting product to room temperature using non-cooling, for at least 10 s. Morphological characteristics of the hydrated amorphous alumina and Y-alumina in the form of spherical particles are listed in Table 1. To obtain (y; -Oxide oxide with the morphological and particle size specified in Table 1, it is necessary to heat treatment by instantly raising the temperature of the starting compound from room temperature to the processing temperature. The device used for the heat treatment should be set to the processing temperature and the original compound at room temperature should be instantly introduced into the device. at 550 -, instantly entering it into the device for the second heat treatment, in which the required temperature is set in the mind, the processing can be started similarly from the initial temperatures of the powders in the range from room temperature to the temperature of formation of the J-phase, i.e. formation temperatures of the starting compounds, including mixtures of α-alumina and crystalline hydrated aluminum oxide, with their direct introduction into the heat treatment system, previously set to the desired temperature. After processing at the required temperature and for a specified time, the powder must be kept at a room temperature, while it is necessary that the cooling process be short (on the order of a few seconds, usually 10 s). By carrying out the process under the proposed conditions, it is possible to obtain α-alumina, in mixtures of C ,, -alumina consisting of delta and / or theta alumina, the content of the phase is 70 wt.%. For the implementation of the proposed method Lyuby can be used; -f: hLHYA -. ;;. G - o: dicky aluminum or a mixture /: 1l of obtaining oi-alumina, provided that they have the indicated in Table. 1 granulometric and morphological characteristics. Hydrated alumina for the proposed method can be obtained from alumini sulphate solutions by hydrolysis at temperatures above 90 ° C (on order), with half a half non-aggregated monodispersed starting compound in the form of spherical particles during the process at concentrations ranging from 2x10 to 5x10 zero aluminum. Example 1: Preparation of starting material. Hydrated alumina (water content corresponds to about 35 mAd) in the amorphous phase in the form of non-aggregated spherical particles with an average linear diameter of d 0.16 µm and a polydispersity index of 1.19 are obtained as aerosol. Nitrogen is used as carrier gas, and secondary aluminum butoxide is used as an aluminum compound. A stream of dry nitrogen at 155 ° C and a flow rate of 250 l / h (as measured at room temperature) carrying 8.9 g / h of secondary aluminum butylate in the form of steam is mixed with a second cold stream of nitrogen at 5 ° C and flow rate 500 l / h (measured at room temperature. The ejector produces an aerosol at 55 ° C. The Reynolds number in the transforming part of the ejector is 2,200. The starting compound particles are perfectly spherical, non-agglomerated and dispersed by water. X-ray analysis of the powders showed that hydrate obtained Oxide alumina is in amorphous form. Preparation of oi-alumina. 10 g of AljOjSli O at room temperature is subjected to instant heat treatment by injecting powder into a horizontal furnace, heated to 1150 ° C and keeping it at this temperature for about 8 minutes 1 °; Then the powder is removed from the oven and cooled for several minutes at room temperature. The characteristics of the obtained powder are given in table. 2. An x-ray analysis of the powder of the obtained product showed that the alumina is completely in the α phase. Example 1a (comparative). 10 g of the starting compound of Example 1 was introduced at room temperature to a heat treatment bath. Further, the process is carried out according to Example 1, but the heat treatment temperature is reached in 6 hours. X-ray analysis of the porous showed that the whole product is in .4-form, but the particles do not retain the morphological and granulometric characteristics of the starting compound, i.e. do not have a spherical shape, tend to be destroyed and subject to significant aggregation and sintering. PRI me R 16 (comparative). 10 g of Al OjSlIjO in example 1 is subjected to processing according to example 1, but the processing time is 2 minutes. An x-ray analysis of the obtained powders showed that the product consists of a mixture of delta-alumina (80 wt.) And (U-alumina and has the characteristics of the starting compound. EXAMPLE 1b (comparative). The process is carried out according to example 1-6 No heat treatment of the wire for 1 min. X-ray analysis showed that nojiy4eH delta is alumina without an fti-phase with the initial characteristics retained, but reduced by about 10 the particle diameter df ,. Example 2 10 g of AljOjSlIjO prepared in Example 1 is subjected to heat / at a temperature of 800 ° C for 4 hours using a two-hour temperature profile, the powder is cooled and removed from the oven (cooling takes place in a few minutes). X-ray analysis showed that the product is oi-luminium (water content 3 wt .). The characteristics of the obtained powder are given in Table 2. Preparation of α-alumina. 5 g of γ-alumina at room temperature was subjected to heat treatment. In Example 1, the characteristics of the obtained ft-alumina are given in Table. 2. PRI me R 2a (comparative). 9 g of u-alumina in example 2 is subjected to heat treatment as in example 1a. The resulting product has characteristics similar to the characteristics of the product of example 1a. Example 3. 5g U-alumina obtained in Example 2, at a temperature of 800 ° C, is subjected to heat treatment according to Example 1. The resulting product has characteristics similar to the characteristics of the product according to example 2. Pr im. The process is carried out as in example 1, however, the heat treatment is carried out at for 1 O s. The resulting product has the characteristics as in the product of example 1, P r and m with p 5. 10 g AljOj-, having d 0.32 μm and the polydispersity index - 1.17, in a spherical QVI non-aggregated form, made in the form of aerosol according Example 1, but the flow rate of dry nitrogen at a temperature of 158 C is 200 l / g, the gas carries 7, g / h of secondary aluminum butoxide, the second gas stream of dry nitrogen is fed at 0 ° C at a rate of 400 l / h, the Reynolds number 1820. Aerosol formation temperature. In the hydrolysis chamber, the contact time is 37 s. The ratio of water to secondary aluminum butylate is equal to the heat treatment mode corresponding to example 3. The characteristics of the resulting product -oi-alumina are given in table. 2. PRI m i r 6. TO g А1 „0, -ZN, O in IV I Z fory spherical and non-aggregated particles having an average diameter c1 of 1.35 μm, the ratio is 1.13, were manufactured. according to example 1, the form of an aerosol under the following conditions: the first gas stream at 15b C is supplied with an ambient flow of 300 l / h, portable 10.7 g / m of secondary Putilag aluminum, the second gas stream has a temperature of 0 ° C and 300 l / h , the temperature of aerosol formation is 78 ° C, the hydrolysis time is b7 s, the molar ratio of water to lure aluminum butylate is 15. The resulting product was processed according to py 1 but Y50 T ° C, t 5. The resulting product is l-alumina, the characteristics of which are given in table. 2. Example7. The process is conducted according to example 6, conduct heat treatment at 125 ° C for 90 s. The characteristics of the obtained product are (γ-alumina, similar to those of the product obtained according to Example 6. PRI mme ip B. Preparation of the starting compound. Solution A1, (S04) with a concentration of 2 to 10 mol / l of aluminum is aged in for one week at 98 ° C until 2 g of A1 Oj ZN ohlichina is formed and the pH of the initial solution is approximately the same after aging the pH is 3. Thus, the product is obtained in the form of spherical non-aggregated monodisperse particles having d 0.53 µm and polydispersity index i 1, j. Preparation of oi-alumina The resulting product was subjected to ts-processing in accordance with Example 1. The ivi-alumina was obtained, the characteristics of which are given in Table 2. The proposed method makes it possible to obtain o-alumina in the form of spherical non-aggregated particles suitable for the manufacture of ceramics. The method of producing spherical O-alumina, which involves calcining the fti-alumina precursor from room temperature or from 830 ° C and subsequent cooling of the product, characterized in that, in order to expand the process Capabilities by using the product to produce ceramics, the precursor (xi-alumina is taken with a water content of 235 wt., a polydispersity index of less than 2, and an average diameter of 0.1-1.5 microns, calcined at 1150-1 ° 50 ° C for not more than 10 minutes, g ohl Duration lead at least for 10s.
    [2]
    2. The method according to p. 1, and t l and h ayusch and the fact that when using as precursor 0 (J-alumina hydrated alumina with an average diameter of O, 37 m, the calcination is 7-10 minutes at a temperature about and 12-18 s at a temperature of about. 1
    [3]
    3. The method of pop, 1, I differ by the fact that when using 1 aluminum oxide as hydrate aluminum oxide with a mean diameter of 0.15 μm as a precursor, the lead temperature is 6–3.5 min at a temperature of about 1150 ° C and 3–15 c at about 1350C, t. A method according to claim 1, characterized in that, when used as the precursor of α-alumina X - alumina with an average diameter of 0.28 µm, calcination is carried out with O-13 at a temperature of about 1350 ° C and 1-2 seconds at about 10 ° C H50 ° C. T a b l and c a
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    同族专利:
    公开号 | 公开日
    EP0188388A2|1986-07-23|
    CA1288575C|1991-09-10|
    KR860005749A|1986-08-13|
    IT1184114B|1987-10-22|
    EP0188388A3|1988-04-06|
    IT8519142D0|1985-01-18|
    ES550980A0|1986-12-01|
    AU585568B2|1989-06-22|
    JPS61256921A|1986-11-14|
    AU5242686A|1986-07-24|
    ES8701690A1|1986-12-01|
    US4818515A|1989-04-04|
    DE3672502D1|1990-08-16|
    KR900004065B1|1990-06-11|
    EP0188388B1|1990-07-11|
    引用文献:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT19142/85A|IT1184114B|1985-01-18|1985-01-18|ALFA ALUMINATES IN THE FORM OF SPHERICAL PARTICLES, NOT AGGREGATED, WITH RESTRIBUTION GRANULOMETRIC RESTRICTED AND OF LESS THAN 2 MICRONS, AND PROCESS FOR ITS PREPARATION|
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