CN1328209C - Prepn of microcrystalline alumina ceramic grain - Google Patents

Prepn of microcrystalline alumina ceramic grain Download PDF

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Publication number
CN1328209C
CN1328209C CNB2005101127250A CN200510112725A CN1328209C CN 1328209 C CN1328209 C CN 1328209C CN B2005101127250 A CNB2005101127250 A CN B2005101127250A CN 200510112725 A CN200510112725 A CN 200510112725A CN 1328209 C CN1328209 C CN 1328209C
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preparation
alumina
suspension
aluminium hydroxide
alpha
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CN1772695A (en
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陈玮
马艳红
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Aluminum Corp of China Ltd
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Aluminum Corp of China Ltd
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Abstract

The present invention relates to a preparation method of microcrystalline alumina ceramic granules, which is characterized in that a preparation process adopts superfine aluminium hydroxide as an original material to prepare alpha-alumine, and the alpha-alumine, aluminum hydroxide and pseudoboehmite are mixed and milled to prepare a suspension. After the suspension is prepared into a gel and is dried and crushed, the gel is sintered, crushed and sieved under the temperature of 1250 DEG-1650 DEG, and the microcrystalline alumina ceramic granules are prepared. Compared with the traditional alumina base abrasive granules, such as white fused alumina, brown fused alumina, etc., the alumina ceramic granules which are prepared by adopting the method of the present invention has the advantages of high hardness, good toughness, favorable abrasive resistance, etc., and a primary crystal is between 200MM to 2 micrometers. The durability of a grinding tool which is prepared by the grinding material is sufficiently increased.

Description

A kind of preparation method of microcrystalline alumina ceramic grain
Technical field
A kind of preparation method of microcrystalline alumina ceramic grain relates to the preparation method of a kind of removing material with the alumina-ceramic abrasive particle, is particularly useful for making the alumina-ceramic grinding product of high-wearing feature.
Background technology
α-Al 2O 3(being commonly called as corundum) is thing phase the most stable in all aluminum oxide, belongs to A2B3 type compound, and trigonal system has fusing point height (reaching 2050 ℃), hardness big (Mohs' hardness reaches 9), and closely (one time the crystal true density reaches 4.01g.cm to structure -3), the physical strength height, chemical property is stable, and goods all have preferably characteristics such as resistibility to acid, alkali.
Based on α-Al 2O 3Characteristics such as hardness height, wear resistance are good, it is widely used as making various removing materials, as the fusion corundum, comprises white fused alumina, brown corundum, high alumina corundum etc.The production of corundum generally will be passed through the fused course of processing.Because through the fused course of processing, aluminum oxide crystal is bigger in the corundum, generally can reach the hundreds of micron, even several millimeter, corundum matter abrasive material has the feature of high rigidity like this, but in the process of grinding, because the hardness height, fragility greatly generally shows as transgranular cracking, and therefore the use properties to grinding tool produces very big negative impact, the toughness that mainly shows as abrasive particle is low, and the wearing quality of grinding tool is not high.Though it is also very high on the alundum hardness, but, be the feint material of corner angle on the microstructure of the prepared material that comes out, so cutting force is not strong because the course of processing is powder sintering technology, can only be used as polishing material and use, and can not use as the abrasive material of the high-strength cutting force of needs.
Summary of the invention
Purpose of the present invention is exactly at the weak point of corundum matter abrasive particle on toughness, the preparation method of the microcrystalline alumina ceramic grain that the grinding tool cutting force that provides a kind of toughness to improve greatly, prepare is strong.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of microcrystalline alumina ceramic grain is characterized in that its preparation process comprises:
A, preparation ultrafine alpha-alumina
Adding is magnesium oxide or the aluminum fluoride of 0.2%-0.5% with the aluminium hydroxide weight ratio in aluminium hydroxide, makes Alpha-alumina at 1100 ℃~1300 ℃ temperature lower calcination, is crushed to D 50Less than 1.0 μ m;
B, preparation aluminium hydroxide and pseudo-boehmite mixture
With the mol ratio of aluminium is that 0.1~5 aluminium hydroxide and pseudo-boehmite mixed grinding are to D 50Less than 1.5 μ m;
C, prepare suspension
By aluminium in the mixture of aluminium in the Alpha-alumina and b step is 0.05~0.8 mol ratio, the Alpha-alumina micro mist is added the b step prepare in the mixture, and adding water, to be mixed with solid weight content be 20%~50% suspension;
D, preparation gelinite particle
In by the suspension of c preparation, add account for total alumina weight in the suspension 2%~35% be selected from one or more mixture in magnesium oxide, ferric oxide, calcium oxide, the silicon oxide; Suspension is heated to 60~90 ℃ again, control pH value is 1~3, stirs and forms gelinite; Gel is broken into the particle of 0.5~1.5mm after the drying in loft drier;
E, preparation microcrystalline alumina ceramic grain
With the gelinite particle 1250 ℃~1650 ℃ sintering temperatures 2~6 hours; According to the requirement fragmentation of abrasive substance, prepare microcrystalline alumina ceramic grain.
Method of the present invention is a basic material with ultrafine aluminium hydroxide, pseudo-boehmite, add the oxide compound that magnesium oxide, ferric oxide, calcium oxide, silicon oxide etc. at high temperature can form the ceramic of compact body with aluminum oxide, through technologies such as sol-gel, drying, fragmentations, can prepare the alumina ceramic-base abrasive material of superior performance.The preparation process of this abrasive material is because through sol-gel process, can guarantee the homogeneity of various chemical ingredientss in the abrasive particle, because abrasive particle is to be formed by a large amount of small crystal sintering, on macroscopic view, show as strong cutting force, simultaneously the toughness of abrasive particle improves greatly, and therefore the wearing quality based on the prepared grinding tool that comes out abrasive material and prepare of this technology improves greatly.Advantages such as the toughness of prepared alumina ceramic-base has good toughness for corundum matter abrasive material, the grinding tool wearing quality is good.
Specific embodiments
A kind of preparation method of microcrystalline alumina ceramic grain, it is characterized in that its preparation process is that employing aluminium hydroxide is starting raw material, add and promote to change mutually and suppress additive magnesium oxide or the aluminum fluoride that crystal is grown up, the Alpha-alumina of preparing with by the mixed grinding of ultrafine aluminium hydroxide and pseudo-boehmite, add entry in the mixture after grinding, be mixed with suspension, solids content total in the control suspension is 20%~50%, in suspension, add magnesium oxide again, ferric oxide, calcium oxide, in the silicon oxide one or more, can at high temperature form the additive of ceramic of compact sintered compact with aluminum oxide, additive can add with the solid form, also can add corresponding salt, behind high temperature sintering, salt is transformed into corresponding oxide compound, add oxide compound thing weight and account for 2%~35% of total alumina weight in the suspension, in suspension, add mineral acid, and heating is prepared into gelinite, with the gelinite drying, after the fragmentation, sintering temperature at 1250 ℃~1650 ℃, particle behind the sintering passes through fragmentation again, screening makes the raw material for preparing grinding tool.The steps include: a, preparation ultrafine alpha-alumina: adding weight ratio in aluminium hydroxide is magnesium oxide or the aluminum fluoride of 0.2%-0.5%, makes Alpha-alumina at 1100 ℃~1300 ℃ temperature lower calcination, is crushed to D 50Less than 1.0 μ m; B, preparation aluminium hydroxide and pseudo-boehmite mixture: with the mol ratio of aluminium is that 0.1~5 aluminium hydroxide and pseudo-boehmite mixed grinding are to D 50Less than 1.5 μ m; C, prepare suspension: by aluminium in the mixture of aluminium in the Alpha-alumina and b step is 0.05~0.8 mol ratio, the Alpha-alumina micro mist is added the b step prepare in the mixture, and adding water, to be mixed with solid weight content be 20%~50% suspension; D, preparation gelinite particle: in by the suspension of c preparation, add account for total alumina weight in the suspension 2%~35% be selected from one or more mixture in magnesium oxide, ferric oxide, calcium oxide, the silicon oxide; Suspension is heated to 60~90 ℃ again, control pH value is 1~3, stirs and forms gelinite; Gel is broken into the particle of 0.5~1.5mm after the drying in loft drier; E, preparation microcrystalline alumina ceramic grain: with the gelinite particle 1250 ℃~1650 ℃ sintering temperatures 2~6 hours; According to the requirement fragmentation of abrasive substance, prepare microcrystalline alumina ceramic grain.
The prepared alumina ceramic grain of the present invention has the hardness height for conventional aluminium oxide based abrasive grains such as white fused alumina, brown corundum, good toughness, advantage such as wear resistance is good, crystal at 200nm between the 2 μ m.Wearing quality by the prepared grinding tool of this abrasive material improves greatly.
Embodiment 1
At first the aluminium hydroxide with 500 gram D50<1 μ m adds magnesium oxide 1 gram, aluminum fluoride 2 grams, 1200 ℃ of calcinings 2 hours, the Alpha-alumina for preparing is ground into the micro mist of D50<1 μ m, get Alpha-alumina micro mist 30 grams, ultra-fine ultrafine aluminium hydroxide micro mist 100 grams, pseudo-boehmite 300 grams, in the usefulness small grinder of laboratory, ground 12 hours, add calcium oxide 25 grams in the material after grinding, silicon oxide 45 grams, magnesium oxide 30 grams, and 1000ml water, be mixed with suspension, stir and in suspension dripping hydrochloric acid, up to the pH value 1, obtain gelinite, with gelinite in the laboratory with 90 ℃ of dryings in the loft drier, dried gel is broken into the particle less than 1.0mm in jaw crusher, with the 1400 ℃ of calcinings 2 hours in groom's stove of the particle after the fragmentation, obtain ceramic sintered bodies, the ceramic sintered bodies fragmentation obtains the finished product alumina ceramic grain.
Embodiment 2
At first the aluminium hydroxide with 500 gram D50<1 μ m adds magnesium oxide 1 gram, aluminum fluoride 2 grams, 1100 ℃ of calcinings 2.5 hours, the Alpha-alumina for preparing is ground into the micro mist of D50<1 μ m, ultra-fine ultrafine aluminium hydroxide micro mist 100 grams, pseudo-boehmite 300 grams, with grinding 12 hours in the small grinder, adds entry 500ml in the material after the grinding in the laboratory, silicon oxide 45 grams, be mixed with suspension, the suspension that obtains mixing adds 1g.ml in suspension -1Ca nitrate soln 70ml, 1g.ml -1Magnesium nitrate solution 100ml, dripping hydrochloric acid, up to the pH value 2, and heating obtains gelinite, with gelinite in the laboratory with 90 ℃ of dryings in the loft drier, dried gel is broken into the particle less than 0.5mm in jaw crusher, with the 1250 ℃ of calcinings 4 hours in groom's stove of the particle after the fragmentation, obtain ceramic sintered bodies, fragmentation obtains the finished product alumina ceramic grain.
Embodiment 3
Get Alpha-alumina micro mist 50 grams of preparation among the embodiment 1, ultra-fine ultrafine aluminium hydroxide micro mist 80 grams, ultra-fine calcium oxide 45 grams, micro silica 55 grams, magnesium oxide 40 grams, pseudo-boehmite 350 grams, water 500 grams are mixed with suspension, use in the small grinder in the laboratory and grind 12 hours, the suspension that obtains mixing, 15% dilute hydrochloric acid in suspension, 3, and heating obtains gelinite up to the pH value, with gelinite 90 ℃ of dryings in the usefulness loft drier of laboratory, dried gel is broken into the particle less than 1.5mm in jaw crusher, with the particle after the fragmentation in groom's stove 1650 ℃ the calcining 2 hours, obtain ceramic sintered bodies, ceramic sintered bodies is broken into different granularities, obtains the finished product alumina ceramic grain.
Embodiment 4
At first the aluminium hydroxide with 500 gram D50<1 μ m adds magnesium oxide 1 gram, aluminum fluoride 2 grams, 1300 ℃ of calcinings 2 hours, the Alpha-alumina for preparing is ground into the micro mist of D50<1 μ m, get Alpha-alumina micro mist 30 grams of preparing, ultra-fine ultrafine aluminium hydroxide micro mist 60 grams, calcium chloride 45 grams, magnesium nitrate 50 grams, pseudo-boehmite 400 grams, water 500 grams, be mixed with suspension, with grinding 12 hours in the small grinder, the suspension that obtains mixing drips nitric acid in suspension in the laboratory, up to the pH value 2, and heating, obtain gelinite, with gelinite 90 ℃ of dryings in the usefulness loft drier of laboratory, dried gel is broken into the particle less than 1.0mm in jaw crusher, with the particle after the fragmentation in groom's stove 1350 ℃ the calcining 5 hours, obtain ceramic sintered bodies, the ceramic sintered bodies fragmentation obtains the finished product alumina ceramic grain.
Embodiment 4
Get Alpha-alumina micro mist 30 grams of preparation among the embodiment 1, ultra-fine ultrafine aluminium hydroxide micro mist 50 grams, magnesium nitrate 80 grams, pseudo-boehmite 400 grams, water 500 grams are mixed with suspension, use in the small grinder in the laboratory and grind 12 hours, the suspension that obtains mixing, in suspension, drip nitric acid, up to the pH value between 1~3, and the heating, obtain gelinite, with gelinite in the laboratory with 80 ℃ of dryings in the loft drier, dried gel is broken into the particle less than 1.5mm in jaw crusher, with the 1250 ℃ of calcinings 6 hours in groom's stove of the particle after the fragmentation, obtain ceramic sintered bodies, the ceramic sintered bodies fragmentation obtains the finished product alumina ceramic grain.
Embodiment 5
Get Alpha-alumina micro mist 30 grams of preparation among the embodiment 1, ultra-fine ultrafine aluminium hydroxide micro mist 50 grams, calcium chloride 80 grams, pseudo-boehmite 400 grams, water 500 grams are mixed with suspension, use in the small grinder in the laboratory and grind 12 hours, the suspension that obtains mixing, in suspension, drip nitric acid, up to the pH value between 2-3, and the heating, obtain sol system, with gelinite in the laboratory with 80 ℃ of dryings in the loft drier, dried gel is broken into the particle less than 0.5mm in jaw crusher, with the 1250 ℃ of calcinings 5 hours in groom's stove of the particle after the fragmentation, obtain ceramic sintered bodies, ceramic sintered bodies is broken into alumina ceramic grain.

Claims (2)

1. the preparation method of a microcrystalline alumina ceramic grain is characterized in that its preparation process comprises:
A, preparation ultrafine alpha-alumina
Adding is magnesium oxide or the aluminum fluoride of 0.2%-0.5% with the aluminium hydroxide weight ratio in aluminium hydroxide, makes Alpha-alumina at 1100 ℃~1300 ℃ temperature lower calcination, is crushed to D 50Less than 1.0 μ m;
B, preparation aluminium hydroxide and pseudo-boehmite mixture
With the mol ratio of aluminium is that 0.1~5 aluminium hydroxide and pseudo-boehmite mixed grinding are to D 50Less than 1.5 μ m;
C, prepare suspension
In the mol ratio of aluminium in the mixture of aluminium in the Alpha-alumina and b step is 0.05~0.8 ratio, the Alpha-alumina micro mist is added in the mixture of b step preparation, and adding water, to be mixed with solid weight content be 20%~50% suspension;
D, preparation gelinite particle
In by the suspension of c preparation, add account for total alumina weight in the suspension 2%~35% be selected from one or more oxide compound in magnesium oxide, ferric oxide, calcium oxide, the silicon oxide; Add hot suspension to 60~90 ℃, control pH value is 1~3, stirs the formation gelinite; Gel is broken into the particle of 0.5~1.5mm after the drying in loft drier;
E, preparation microcrystalline alumina ceramic grain
With the gelinite particle 1250 ℃~1650 ℃ sintering temperatures 2~6 hours; According to the requirement fragmentation of abrasive substance, prepare microcrystalline alumina ceramic grain.
2. the preparation method of a kind of microcrystalline alumina ceramic grain according to claim 1 is characterized in that the aluminium hydroxide that adopts is ultrafine aluminium hydroxide.
CNB2005101127250A 2005-10-12 2005-10-12 Prepn of microcrystalline alumina ceramic grain Active CN1328209C (en)

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Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318827B (en) * 2008-06-20 2010-12-15 江苏苏北砂轮厂有限公司 Firing method for manufacturing ceramic minicrystal grinding tool
CN102070169A (en) * 2010-12-15 2011-05-25 中国铝业股份有限公司 Preparation method of low-sodium active aluminum oxide
CN102432317A (en) * 2011-09-20 2012-05-02 宜兴市九荣特种陶瓷有限公司 Microcrystalline alumina wear resistant ceramics and preparation method thereof
CN103387385B (en) * 2013-07-30 2014-12-17 宁波厨聚厨房科技有限公司 Ceramic grinding head material for grinder
CN105819833B (en) * 2015-01-04 2019-02-05 江门市凯斯特尔实业有限公司 A kind of preparation method from sharp type Fine Grain Alumina Ceramics abrasive grain
CN105036712A (en) * 2015-05-29 2015-11-11 贵州格勒尔高新材料有限公司 Preparation method of microcrystalline corundum abrasive material
CN105622071A (en) * 2015-12-23 2016-06-01 山东大学 Alpha-Al2O3 ceramic particles containing lamellar microcrystals as well as preparation method for ceramic particles and application of ceramic particles
CN105668599B (en) * 2016-01-14 2018-08-10 洛阳三睿宝纳米科技有限公司 A kind of nano aluminium oxide polishing material and preparation method thereof
CN106431364B (en) * 2016-09-09 2019-08-02 苏州创元新材料科技有限公司 The preparation method of high temperature sintering ceramic alumina abrasive material
CN106518117A (en) * 2016-10-07 2017-03-22 常州市鼎日环保科技有限公司 Superhard ceramic abrasive material preparation method
CN111320465B (en) * 2020-03-25 2022-01-14 山东大学 Alumina-based microcrystalline ceramic particles and preparation method and application thereof
CN112939587B (en) * 2021-02-09 2023-03-03 洛阳润宝研磨材料有限公司 Preparation method of high-density nano ceramic grinding material

Citations (3)

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Publication number Priority date Publication date Assignee Title
US4314827A (en) * 1979-06-29 1982-02-09 Minnesota Mining And Manufacturing Company Non-fused aluminum oxide-based abrasive mineral
US4623364A (en) * 1984-03-23 1986-11-18 Norton Company Abrasive material and method for preparing the same
CN1189475A (en) * 1997-12-16 1998-08-05 武汉工业大学 Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4314827A (en) * 1979-06-29 1982-02-09 Minnesota Mining And Manufacturing Company Non-fused aluminum oxide-based abrasive mineral
US4623364A (en) * 1984-03-23 1986-11-18 Norton Company Abrasive material and method for preparing the same
CN1189475A (en) * 1997-12-16 1998-08-05 武汉工业大学 Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball

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