CN107226686A - A kind of Deep processing of minerals high-strength in-situ toughened aluminum oxide mill ball and preparation method thereof - Google Patents

A kind of Deep processing of minerals high-strength in-situ toughened aluminum oxide mill ball and preparation method thereof Download PDF

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CN107226686A
CN107226686A CN201710440729.4A CN201710440729A CN107226686A CN 107226686 A CN107226686 A CN 107226686A CN 201710440729 A CN201710440729 A CN 201710440729A CN 107226686 A CN107226686 A CN 107226686A
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aluminum oxide
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oxide
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mill ball
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CN107226686B (en
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王俊甫
伯恩哈德·克莱因
周雄
宋书明
廖建中
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King's Ceramics & Chemicals Co Ltd
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract

The invention discloses a kind of Deep processing of minerals high-strength in-situ toughened aluminum oxide mill ball and preparation method thereof, using aluminum oxide as main material, using zirconium silicate, zirconium oxide, yittrium oxide, calcium carbonate, magnesium carbonate, potassium carbonate, sodium carbonate as sintering aid, by suitable proportioning, it is spray-dried after ball milling, obtains raw material powder.After being configured to microballoon through bowling machine, sintered within 10 20 hours in 1450 degree to 1500 degree sintering, obtain the alumina ceramic grinding ball of high-intensity high-tenacity.It is mainly used in ultra-large type in industrial mine, energy density is higher than 450Kw/m3In horizontal sand mill.The zirconium oxide produced using zirconium silicate decomposition in situ carries out toughness reinforcing to aluminum oxide, pass through nano alumina powder jointed introducing simultaneously, silica produced by fully erased decomposition, so as to reach raising toughness of material, increases substantially the purpose of the compression strength of abrasive media.

Description

A kind of Deep processing of minerals high-strength in-situ toughened aluminum oxide mill ball and its preparation Method
Technical field
The present invention relates to the preparation of alumina ceramic grinding ball, it is related to for ultra-large type in industrial mine, energy density is higher than 450Kw/m3Alumina ceramic grinding ball in horizontal sand mill.
Background technology
Mill ball is widely used in the industries such as mineral products, metallurgy, chemical industry, food, building materials, by the collision of mill ball, friction, Raw material is crushed and mixed by the various ways such as rolling, extruding.The quality of mill ball has a strong impact on production efficiency and product quality.
In recent years, the exploitation developed rapidly with low-grade mineral products of superfine powder technique, have greatly driven mill ball The exploitation and production of medium.Conventional abrasive media has steel, quartz, glass, aluminum oxide, zirconium oxide etc..Aluminum oxide is as one kind The relatively broad ceramic raw material of originating of low cost, has fragility high, the bad limitation of ductility, merely using oxygen in performance Change aluminium production abrasive media, broken situation easily occurs in the energy mill run at high speed for product；And zirconium oxide is as tough Property relatively good ceramic raw material, good toughening effect can be played to alumina material after addition.
China Patent Publication No. CN101143783A, discloses a kind of Zirconium oxide plasticizing mullite ceramic material and preparation side Method, uses zirconium silicate and Α phase aluminas for matrix, with modern toughness reinforcing and enhancing technology, adds yittrium oxide, magnesia, oxidation Calcium and titanium oxide are mineralizer, and additional mullite makees crystal seed.Modified activeness and quietness, using equal pressing forming technology, makes green With uniformity and compactness, constant-pressure and high-temperature drawer kiln one-time sintering technology is used in sintering process, temperature is uniform and cost is low, The present invention is compared with alumina ceramic material, and it has high intensity, high tenacity, and high-wear resistance, simple production process burns till temperature Degree significantly declines, and reaches energy-saving purpose.Its technical scheme discloses zirconium silicate and aluminum oxide and discloses oxidation Yttrium, magnesia, calcium oxide and titanium oxide are as mineralizer, and it also decomposes Zirconium oxide plasticizing using in-situ reaction, but wherein low Zirconium silicate decomposition efficiency is low under the conditions of temperature, and silica produced by decomposition exists with free state, mainly with crystalline substances such as cristobalites Phase form is present in material, silica low intensity, the poor toughness of free state, and can be because of crystalline phase in high-speed friction adstante febre Change and expand, cause ball to be situated between broken, cause structural stability poor, so as to cause toughness and resistant to breakage ability to reduce.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of middle low temperature control zircon sand decomposition in situ Zirconium oxide plasticizing Aluminum oxide, introduces zirconium dioxide, while by adding nano aluminium oxide, fully erased point on a small quantity by the zirconium silicate of low cost Free silica produced by solution, improves the overall flexibility of material and the Deep processing of minerals high-strength in-situ of resistant to breakage ability Toughened aluminum oxide mill ball and preparation method thereof.
To realize the object of the invention, there is provided following technical scheme：A kind of Deep processing of minerals high-strength in-situ toughness reinforcing oxygen Change aluminium mill ball, material powder includes following component by mass percentage：Host material：Aluminum oxide 60%-85%, zirconium silicate 5%-25%；It is characterized in that adding sintering aid：Zirconium oxide 1%-5%, yittrium oxide 0.5%-3%, calcium carbonate 0.5%-5%, magnesium carbonate 0.5%-5%, potassium carbonate 0.5%-5%；Inducing agent：Nano aluminium oxide 1%-5%.
To realize the object of the invention, there is provided a kind of Deep processing of minerals high-strength in-situ toughness reinforcing as claimed in claim 1 Alumina ceramic grinding ball preparation method, it is characterised in that comprise the following steps：By host material：Aluminum oxide 60%-85%, zirconium silicate 5%-25%；It is characterized in that adding sintering aid：Zirconium oxide 1%-5%, yittrium oxide 0.5%-3%, calcium carbonate 0.5%-5%, magnesium carbonate 0.5%-5%, potassium carbonate 0.5%-5%；Inducing agent：After nano aluminium oxide 1%-5% material powder mixing, water is added mixed through ball mill Material, machine for cutting charge into pieces grinding obtains satisfactory slurry, spray-dried to obtain raw material powder, and element is obtained by bowling machine shaping Base ball；Biscuit ball warp oversintering is obtained to the toughened aluminum oxide ball of compact high-strength degree high abrasion.
Preferably, sintering process is characterized as, with 100C/min is warming up to 10000C, then 2/min0C is warming up to sintering temperature Spend 1450-15000C, is incubated 3-5 hours, then naturally cools to room temperature.
Preferably, material powder：Water：Mill ball ratio is：1：1.5：3.
Preferably, biscuit bulb diameter is 1 ~ 2mm.
Preferably, prepared toughened aluminum oxide mill ball, density is 3.8-4.0g/cm3, Vickers hardness is 1200- 1350Gpa, fracture toughness is 2.8-3.8 MPa m1/2, crushing strength is 1800-2000N, is 1-2g/hr kg, band from abrasion Material abrasion are 1-2g/hr kg.
The key problem in technology of the present invention is：Using commercial alumina and zirconium silicate as host material, by zirconium silicate in it is low The lower decomposition in situ of temperature produces zirconium oxide and carries out toughness reinforcing to alumina material.By introducing, special auxiliary agent and high degree of dispersion are uniform Nano aluminium oxide inducing agent, using the nano effect of its high activity, just start to capture the silicon in zirconium silicate at a lower temperature Oxygen tetrahedron group, induces zirconium silicate decomposition and mullite is mutually formed, and is to reduce the decomposition temperature of zirconium silicate first, reaches silicic acid Zirconium starts the purpose decomposed under middle low temperature, and second be silica phase is reacted away once being formed, it is to avoid free state titanium dioxide The cenotype of the residual of silicon phase, nanometer inducing agent and silica formation is uniformly distributed between main phase grain, forms stable structure, from And reach the target of fast low temperature zirconium silicate decomposition in situ Zirconia reinforced alumina.
Beneficial effect of the present invention：Low raw-material cost of the present invention, manufacture craft is simple, realizes the silicic acid under middle cryogenic conditions Zirconium decomposition in situ, and the residual of free state silica phase is avoided, Stability Analysis of Structures, toughening effect substantially, is adapted to industrialization Using.
Specific implementation method
Embodiment 1：
Quality of alumina percentage is 60%, and zirconium silicate mass percent is 25%, and yittrium oxide mass percent is 3%, nanometer Quality of alumina percentage is 5%, and calcium carbonate mass percent is 0.5%, and potassium carbonate mass percent is 5%, zirconium oxide quality Percentage is 1%, and magnesium carbonate mass percent is 0.5%.
After above material powder is mixed in proportion, water and mill ball are added, ratio is:Raw material powder：Water：Mill ball ratio Example be（1：1.5：3）.Well mixed slurry is obtained through 6 hours of ball milling, is then met through machine for cutting charge into pieces 3 hours of grinding It is required that slurry, it is spray-dried to obtain raw material powder.Raw material powder and water are sprayed into bowling machine, 2mm is obtained by bowling machine shaping The biscuit ball of left and right diameter.Biscuit ball warp oversintering is obtained into zirconium silicate ball.Sintering process is, with 100C/min is warming up to 10000C, then 20C/min is warming up to sintering temperature 14500C, is incubated 3 hours, then naturally cools to room temperature.Prepared Toughened aluminum oxide mill ball, density is 3.9g/cm3, Vickers hardness is 1250Gpa, and fracture toughness is 3.2 MPa m1/2, pressure Broken intensity is 1800N, is 1.0g/hr kg from abrasion, and strip abrasion are 1.2g/hr kg.
Embodiment 2：
Quality of alumina percentage is 70%, and zirconium silicate mass percent is 17%, and yittrium oxide mass percent is 2%, nanometer Quality of alumina percentage is 2%, and calcium carbonate mass percent is 5%, and potassium carbonate mass percent is 0.5%, zirconium oxide quality Percentage is that 1.5 %. magnesium carbonate mass percents are 2%.
After above material powder is mixed in proportion, water and mill ball are added, ratio is:Raw material powder：Water：Mill ball ratio Example be（1：1.5：3）.Well mixed slurry is obtained through 6 hours of ball milling, is then met through machine for cutting charge into pieces 3 hours of grinding It is required that slurry, it is spray-dried to obtain raw material powder.Raw material powder and water are sprayed into bowling machine, 2mm is obtained by bowling machine shaping The biscuit ball of left and right diameter.Biscuit ball warp oversintering is obtained into zirconium silicate ball.Sintering process is, with 100C/min is warming up to 10000C, then 20C/min is warming up to sintering temperature 15000C, is incubated 4 hours, then naturally cools to room temperature.Prepared Zirconium silicate grinding ball, density is 3.7g/cm3, Vickers hardness is 1200Gpa, and fracture toughness is 3.0 MPa m1/2, crushing is by force Spend for 1600N, be 1.2g/hr kg from abrasion, strip abrasion are 1.3g/hr kg.
Embodiment 3 ~ 6, it is as shown in the table：
Aluminum oxide Zirconium silicate Yittrium oxide Nano aluminium oxide Calcium carbonate Potassium carbonate Zirconium oxide Magnesium carbonate
Embodiment 3 65 20 2 2.5 1.5 2 5 2
Embodiment 4 77 15 1.5 1.5 1 0.5 1 2.5
Embodiment 5 80 10 1 3 2 0.5 0.5 3
Embodiment 6 85 5 0.5 1 1 1 1.5 5

Claims (6)

1. a kind of Deep processing of minerals high-strength in-situ toughened aluminum oxide mill ball, by mass percentage material powder include with Lower component：Host material：Aluminum oxide 60%-85%, zirconium silicate 5%-25%；It is characterized in that adding sintering aid：Zirconium oxide 1%- 5%th, yittrium oxide 0.5-3%, calcium carbonate 0.5%-5%, magnesium carbonate 0.5%-5%, potassium carbonate 0.5%-5%；Inducing agent：Nano aluminium oxide 1%-5%。
2. a kind of Deep processing of minerals as claimed in claim 1 high-strength in-situ toughened aluminum oxide mill ball preparation method, its It is characterised by comprising the following steps：By host material：Aluminum oxide 60%-85%, zirconium silicate 5%-25%；It is characterized in that adding sintering Auxiliary agent：Zirconium oxide 1%-5%, yittrium oxide 0.5%-3%, calcium carbonate 0.5%-5%, magnesium carbonate 0.5%-5%, potassium carbonate 0.5%-5%；Induce Agent：After nano aluminium oxide 1%-5% material powder mixing, water is added through ball mill batch mixing, machine for cutting charge into pieces grinding is met the requirements Slurry, it is spray-dried to obtain raw material powder, by bowling machine shaping obtain biscuit ball；Biscuit ball warp oversintering is obtained The toughened aluminum oxide ball of compact high-strength degree high abrasion.
3. a kind of Deep processing of minerals according to claim 2 high-strength in-situ toughened aluminum oxide mill ball preparation method, It is characterized in that sintering process is characterized as, with 100C/min is warming up to 10000C, then 2/min0C is warming up to sintering temperature 1450- 15000C, is incubated 3-5 hours, then naturally cools to room temperature.
4. a kind of Deep processing of minerals according to claim 2 high-strength in-situ toughened aluminum oxide mill ball preparation method, It is characterized in that material powder：Water：Mill ball ratio is：1：1.5：3.
5. a kind of Deep processing of minerals according to claim 2 high-strength in-situ toughened aluminum oxide mill ball preparation method, It is characterized in that biscuit bulb diameter is 1 ~ 2mm.
6. a kind of Deep processing of minerals according to claim 2 high-strength in-situ toughened aluminum oxide mill ball preparation method, It is characterized in that prepared toughened aluminum oxide mill ball, density is 3.8-4.0g/cm3, Vickers hardness is 1200- 1350Gpa, fracture toughness is 2.8-3.8 MPa m1/2, crushing strength is 1800-2000N, is 1-2g/hr kg, band from abrasion Material abrasion are 1-2g/hr kg.
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CN107814560A (en) * 2017-09-30 2018-03-20 江苏金石研磨有限公司 A kind of ceramic grinding ball rolls shaping composite fortifier and preparation method thereof and its application method
CN108298959A (en) * 2017-12-19 2018-07-20 江苏金石研磨有限公司 A kind of liquid condition shaping method of ceramic grinding ball
CN108821789A (en) * 2018-07-30 2018-11-16 界首市鑫全龙粮食机械购销有限公司 A kind of cornmill low-temperature sintered ceramics mill ball
CN108821753A (en) * 2018-07-30 2018-11-16 界首市鑫全龙粮食机械购销有限公司 A kind of wear-resisting mill ball of cornmill
CN111607360A (en) * 2020-06-02 2020-09-01 无锡晨旸科技股份有限公司 Grinding material for large-diameter silicon wafer and production method thereof
CN112250335A (en) * 2020-11-02 2021-01-22 赵生荣 Energy-saving recovery-based method for manufacturing inert filler balls of waste slag
CN112723858A (en) * 2020-12-28 2021-04-30 嘉兴纳美新材料有限公司 Formula and production process of low-cost alumina ceramic ball
CN114538920A (en) * 2022-03-17 2022-05-27 浙江金琨西立锆珠有限公司 Preparation method of high-toughness high-hardness zirconium lanthanum aluminum composite grinding medium
CN114702307A (en) * 2022-01-14 2022-07-05 洛阳索莱特材料科技有限公司 Preparation method of compact alumina ceramic product
CN115340369A (en) * 2022-10-18 2022-11-15 山东合创明业精细陶瓷有限公司 Ternary complex phase wear-resistant ceramic ball and preparation method thereof
CN118439850A (en) * 2024-07-05 2024-08-06 淄博启明星新材料股份有限公司 Alumina-based ceramic polyhedral grinding medium and preparation method thereof

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Cited By (14)

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Publication number Priority date Publication date Assignee Title
CN107814560A (en) * 2017-09-30 2018-03-20 江苏金石研磨有限公司 A kind of ceramic grinding ball rolls shaping composite fortifier and preparation method thereof and its application method
CN108298959A (en) * 2017-12-19 2018-07-20 江苏金石研磨有限公司 A kind of liquid condition shaping method of ceramic grinding ball
CN108298959B (en) * 2017-12-19 2021-01-29 江苏金石研磨有限公司 Liquid forming method of ceramic grinding ball
CN108821753A (en) * 2018-07-30 2018-11-16 界首市鑫全龙粮食机械购销有限公司 A kind of wear-resisting mill ball of cornmill
CN108821789A (en) * 2018-07-30 2018-11-16 界首市鑫全龙粮食机械购销有限公司 A kind of cornmill low-temperature sintered ceramics mill ball
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CN112250335A (en) * 2020-11-02 2021-01-22 赵生荣 Energy-saving recovery-based method for manufacturing inert filler balls of waste slag
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CN118439850B (en) * 2024-07-05 2024-10-11 淄博启明星新材料股份有限公司 Alumina-based ceramic polyhedral grinding medium and preparation method thereof

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