CN105924213A - Method for preparing lightweight porous aluminum phosphate-silicon carbide ceramic balls - Google Patents

Method for preparing lightweight porous aluminum phosphate-silicon carbide ceramic balls Download PDF

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CN105924213A
CN105924213A CN201610283637.5A CN201610283637A CN105924213A CN 105924213 A CN105924213 A CN 105924213A CN 201610283637 A CN201610283637 A CN 201610283637A CN 105924213 A CN105924213 A CN 105924213A
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silicon carbide
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aluminum phosphate
temperature
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CN105924213B (en
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白佳海
高杰
杜庆洋
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Shandong University of Technology
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Abstract

The invention relates to a method for preparing lightweight porous aluminum phosphate-silicon carbide ceramic balls. The method is characterized in comprising the following steps: (1) silicon carbide powder, alumina powder, aluminum dihydrogen phosphate powder and frit powder are subjected to dry mixing according to a certain ratio; (2) granulation and molding are carried out, such that a cylindrical blank is prepared; (3) the blank is dried for 5h under a temperature of 70 DEG C, and is placed into an alumina crucible with a semispherical-shaped inner bottom; the blank heated to a temperature of 150 DEG C in an air atmosphere with a speed of 5 DEG C/min; the temperature is maintained for 2h; the blank is heated to a temperature of 380 DEG C with a speed of 10-20 DEG C/min, and the temperature is maintained for 1h; the blank is heated to a temperature of 680 DEG C with a speed of 1 DEG C/min, and the temperature is maintained for 2h; the blank is heated to a temperature of 1150 DEG C with a speed of 5 DEG C/min, and the temperature is maintained for 2h; and the product is naturally cooled to room temperature, such that the lightweight porous aluminum phosphate-silicon carbide ceramic balls are obtained.

Description

A kind of preparation method of light porous aluminum phosphate silicon carbide ceramics ball
Technical field
The present invention is to provide the preparation method of a kind of light porous aluminum phosphate silicon carbide ceramics ball, belong to special cermacis Technical field of material.
Background technology
Porous alumionphosphate (AlPO4) application in the industrial production of carborundum (SiC) Ceramic Balls widely, Ke Yizuo For catalyst carrier, chemical filler, insulation and refractory material etc..As carrier of photocatalyst and other liquid phase reactor catalyst Carrier, and as in water during the adsorbent of noxious substance, in order to ensure, there is efficient catalytic effect and (or) adsorption efficiency, Often requiring that porous ceramic ball is in suspended state in water, this is accomplished by preparing a kind of light porous ceramic ball.At present, domestic The outer spheroid mainly using the Organic substance that easily burning is lost to make is as " core " of spherical base substrate, and then by burning till, removing is spherical to be had Machine " core ", thus prepare a kind of suspensible porous ceramics hollow ball.The shortcoming of the method is: molding is more difficult, and organic Thing burns during losing, and is easily caused pottery cracking or destroys, reducing the yield rate of product；Additionally, this technical process is more complicated, Relatively costly, deficiency in economic performance, easily pollute environment.In order to overcome an above-mentioned difficult problem, invention provides a kind of efficiently, simple, The preparation method of light porous aluminum phosphate silicon carbide ceramics ball safe and reliable, easily operated, with low cost.
Summary of the invention
The technology of the present invention provides a kind of light porous phosphoric acid efficient, simple, safe and reliable, easily operated, with low cost The preparation method of aluminium silicon carbide Ceramic Balls, its technical scheme is:
The preparation method of a kind of light porous aluminum phosphate silicon carbide ceramics ball, it is characterised in that use following steps: (1) is carbon SiClx powder, alumina powder, biphosphate aluminium powder, frit powder enters according to the ratio that mass ratio is 2:1:3.11:0.03 Row is dry mixed；Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit；(2) add dense Degree be the poly-vinyl alcohol solution of 8 wt% as binding agent, the addition of binding agent is the 5% of blank gross mass；Then pelletize, one-tenth Type, prepares cylindric base substrate；(3) after 70 DEG C of dry base substrates 5 hours, it is the oxidation that semicircle is spherical that base substrate is put into inner bottom part In aluminum crucible, under air atmosphere, heat to 150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, then with 10-20 DEG C/speed of min heats to 380 DEG C and is incubated 1 hour, then heats to 680 with the speed of 1 DEG C/min DEG C and be incubated 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, natural cooling subsequently To room temperature, i.e. prepare light porous aluminum phosphate silicon carbide ceramics ball.
The preparation method of described a kind of light porous aluminum phosphate silicon carbide ceramics ball, it is characterised in that: in step (1) Silicon carbide powder and the mean diameter of oxide powder be all 0.6 micron, aluminium dihydrogen phosphate powder average particle size is 0.5 micron, The mean diameter of frit powder is 0.7 micron.
The preparation method of described a kind of light porous aluminum phosphate silicon carbide ceramics ball, it is characterised in that: in step (2) Molding refer to carry out dry-pressing formed to powder body, briquetting pressure is 10-25MPa.
Fig. 1 is the photo figure that light porous aluminum phosphate silicon carbide ceramics ball prepared by the technology of the present invention floats in water； As can see from Figure 1: aluminum phosphate silicon carbide ceramics ball prepared by this technological invention floats in water, and aluminum phosphate carbon is described The bulk density of SiClx Ceramic Balls is less than the density of water, and the aluminum phosphate silicon carbide ceramics that i.e. prepared by this technological invention belongs to lightweight Porous ceramics.
The principle of this technological invention is as follows:
Utilizing aluminium dihydrogen phosphate melting at a lower temperature is liquid, and the most coagulable performance makes Base substrate spontaneously forms as spheroid in sintering process, concrete principle is as follows: aluminium dihydrogen phosphate is heated to 150 DEG C, insulation 2 After hour, aluminium dihydrogen phosphate is changed into as liquid, is then heated rapidly to 380 DEG C and is incubated 1 hour, its objective is to make various Raw material forms the viscous body that a kind of viscosity is the biggest at such a temperature.The effect adding frit is on the one hand can to promote raw materials melt For the viscous body that a kind of viscosity is the biggest, on the other hand surface tension can also be increased so that viscous physical ability spontaneously forms as spheroid. During being heated slowly to 680 DEG C, aluminium dihydrogen phosphate is gradually solidified as solid；In temperature-rise period, aluminium dihydrogen phosphate can be decomposed into Aluminum phosphate, steam and phosphoric acid, the phosphoric acid of generation can react with magnesium carbonate and generate aluminum phosphate carborundum, and steam and dioxy Change carbon etc. and there is the effect of pore-forming, thus can prepare light porous aluminum phosphate silicon carbide ceramics.
Detailed description of the invention
Embodiment 1
Silicon carbide powder, alumina powder, biphosphate aluminium powder, frit powder is 2:1:3.11:0.03 according to mass ratio Ratio be dry mixed；Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit； The mean diameter controlling silicon carbide powder and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, The mean diameter of frit powder is 0.7 micron；Add concentration be the poly-vinyl alcohol solution of 8 wt% as binding agent, binding agent Addition is the 5% of blank gross mass；Then pelletize, with 10MPa pressure dry-pressing formed, prepare cylindric base substrate；Do at 70 DEG C Dry base substrate is after 5 hours, base substrate is put in inner bottom part is the alumina crucible that semicircle is spherical, with 5 DEG C/min under air atmosphere Speed heat to 150 DEG C and be incubated 2 hours, then heat to 380 DEG C with the speed of 10 DEG C/min and be incubated 1 Individual hour, then heat to 680 DEG C with the speed of 1 DEG C/min and be incubated 2 hours, finally adding with the speed of 5 DEG C/min Heat is warmed up to 1150 DEG C and is incubated 2 hours, naturally cools to room temperature subsequently, i.e. prepares light porous aluminum phosphate and carborundum Ceramic Balls.The bulk density recording porous ceramic ball with Archimedes method is 0.93 g/cm3, open pore rate is 38 %.Use XRD It is aluminum phosphate carborundum that analysis records the crystalline phase of Ceramic Balls.
Embodiment 2
Silicon carbide powder, alumina powder, biphosphate aluminium powder, frit powder is 2:1:3.11:0.03's according to mass ratio Ratio is dry mixed；Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit；Control The mean diameter of preparing silicon carbide powder and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, molten The mean diameter of block powder is 0.7 micron；Adding concentration is that the poly-vinyl alcohol solution of 8 wt% is as binding agent, adding of binding agent Dosage is the 5% of blank gross mass；Then pelletize, with 20MPa pressure dry-pressing formed, prepare cylindric base substrate；It is dried at 70 DEG C After base substrate 5 hours, base substrate is put in inner bottom part is the alumina crucible that semicircle is spherical, with 5 DEG C/min's under air atmosphere Speed heats to 150 DEG C and is incubated 2 hours, then heats to 380 DEG C with the speed of 15 DEG C/min and be incubated 1 Hour, then heat to 680 DEG C with the speed of 1 DEG C/min and be incubated 2 hours, finally heating with the speed of 5 DEG C/min It is warmed up to 1150 DEG C and is incubated 2 hours, naturally cooling to room temperature subsequently, i.e. preparing light porous aluminum phosphate carborundum pottery Porcelain ball.The bulk density recording porous ceramic ball with Archimedes method is 0.93 g/cm3, open pore rate is 36 %.Divide with XRD It is aluminum phosphate and carborundum that analysis records the crystalline phase of Ceramic Balls.
Embodiment 3
Silicon carbide powder, alumina powder, biphosphate aluminium powder, frit powder is 2:1:3.11:0.03's according to mass ratio Ratio is dry mixed；Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit；Control The mean diameter of preparing silicon carbide powder and oxide powder is all 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, The mean diameter of frit powder is 0.7 micron；Add concentration be the poly-vinyl alcohol solution of 8 wt% as binding agent, binding agent Addition is the 5% of blank gross mass；Then pelletize, dry-pressing formed with 25 MPa pressure, prepare cylindric base substrate；Do at 70 DEG C Dry base substrate is after 5 hours, base substrate is put in inner bottom part is the alumina crucible that semicircle is spherical, with 5 DEG C/min under air atmosphere Speed heat to 150 DEG C and be incubated 2 hours, then heat to 380 DEG C with the speed of 20 DEG C/min and be incubated 1 Individual hour, then heat to 680 DEG C with the speed of 1 DEG C/min and be incubated 2 hours, finally adding with the speed of 5 DEG C/min Heat is warmed up to 1150 DEG C and is incubated 2 hours, naturally cools to room temperature subsequently, i.e. prepares light porous aluminum phosphate carborundum Ceramic Balls.The bulk density recording porous ceramic ball with Archimedes method is 0.95g/cm3, open pore rate is 34 %.Divide with XRD It is aluminum phosphate and carborundum that analysis records the crystalline phase of Ceramic Balls.

Claims (3)

1. the preparation method of a light porous aluminum phosphate silicon carbide ceramics ball, it is characterised in that use following steps: (1) Silicon carbide powder, alumina powder, biphosphate aluminium powder, frit powder is the ratio of 2:1:3.11:0.03 according to mass ratio It is dry mixed；Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit；(2) add Concentration be the poly-vinyl alcohol solution of 8 wt% as binding agent, the addition of binding agent is the 5% of blank gross mass；Then pelletize, Molding, prepares cylindric base substrate；(3) after 70 DEG C of dry base substrates 5 hours, it is the oxygen that semicircle is spherical that base substrate is put into inner bottom part Change in aluminum crucible, under air atmosphere, heat to 150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, then with 10-20 DEG C/speed of min heats to 380 DEG C and is incubated 1 hour, then heats to 680 with the speed of 1 DEG C/min DEG C and be incubated 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, natural cooling subsequently To room temperature, i.e. prepare light porous aluminum phosphate silicon carbide ceramics ball.
The preparation method of a kind of light porous aluminum phosphate silicon carbide ceramics ball the most as claimed in claim 1, it is characterised in that: Silicon carbide powder and the mean diameter of oxide powder in step (1) are all 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, the mean diameter of frit powder is 0.7 micron.
The preparation method of a kind of light porous aluminum phosphate silicon carbide ceramics ball the most as claimed in claim 1, it is characterised in that: Molding in step (2) refers to carry out dry-pressing formed to powder body, and briquetting pressure is 10-25MPa.
CN201610283637.5A 2016-05-04 2016-05-04 A kind of preparation method of light porous aluminum phosphate-silicon carbide ceramics ball Expired - Fee Related CN105924213B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109553420A (en) * 2018-12-28 2019-04-02 淄博赛拉米克陶瓷科技有限公司 A kind of preparation method of high porosity silicon carbide-based porous ceramic material
CN116239383A (en) * 2023-05-08 2023-06-09 苏州拓瓷科技有限公司 Silicon carbide ceramic preform and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1091764A (en) * 1993-02-19 1994-09-07 胡小弟 The high temperature compound binding agent
CN102220125A (en) * 2010-04-19 2011-10-19 袁新 Low-density and high-strength silicon-carbide-based fracturing proppant
CN103396150A (en) * 2013-07-30 2013-11-20 河南煤业化工集团研究院有限责任公司 Method for preparing foam ceramic self-insulation wall material by utilizing solid wastes
CN105481464A (en) * 2014-09-19 2016-04-13 青岛百键城环保科技有限公司 Porous refractory material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1091764A (en) * 1993-02-19 1994-09-07 胡小弟 The high temperature compound binding agent
CN102220125A (en) * 2010-04-19 2011-10-19 袁新 Low-density and high-strength silicon-carbide-based fracturing proppant
CN103396150A (en) * 2013-07-30 2013-11-20 河南煤业化工集团研究院有限责任公司 Method for preparing foam ceramic self-insulation wall material by utilizing solid wastes
CN105481464A (en) * 2014-09-19 2016-04-13 青岛百键城环保科技有限公司 Porous refractory material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109553420A (en) * 2018-12-28 2019-04-02 淄博赛拉米克陶瓷科技有限公司 A kind of preparation method of high porosity silicon carbide-based porous ceramic material
CN116239383A (en) * 2023-05-08 2023-06-09 苏州拓瓷科技有限公司 Silicon carbide ceramic preform and preparation method and application thereof
CN116239383B (en) * 2023-05-08 2023-08-15 苏州拓瓷科技有限公司 Silicon carbide ceramic preform and preparation method and application thereof

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