CN107226686B - High-strength in-situ toughening alumina grinding ball for mineral deep processing and preparation method thereof - Google Patents
High-strength in-situ toughening alumina grinding ball for mineral deep processing and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength in-situ toughening alumina grinding ball for mineral deep processing and a manufacturing method thereof. After the mixture is formed into microspheres by a ball rolling machine, the microspheres are sintered for 10 to 20 hours at 1450 to 1500 ℃ to obtain the high-strength and high-toughness alumina grinding balls. Is mainly used for ultra-large industrial mines, and has energy density higher than 450Kw/m3In a horizontal sand mill. The zirconium oxide generated by in-situ decomposition of zirconium silicate is utilized to toughen the aluminum oxide, and simultaneously, the silicon dioxide generated by decomposition is completely removed by introducing the nano aluminum oxide powder, so that the aims of improving the toughness of the material and greatly improving the compressive strength of the grinding medium are fulfilled.
Description
Technical Field
The invention relates to preparation of alumina grinding balls, which are used for ultra-large industrial mines and have energy density higher than 450Kw/m3Alumina grinding balls in a horizontal sand mill.
Background
The grinding balls are widely applied to industries such as mineral products, metallurgy, chemical industry, food, building materials and the like, and the raw materials are crushed and uniformly mixed through various modes such as collision, friction, rolling, extrusion and the like of the grinding balls. The quality of the grinding balls seriously affects the production efficiency and the product quality.
In recent years, the rapid development of the superfine powder process and the development and utilization of low-grade mineral products greatly drive the development and production of grinding ball media. Common grinding media are steel, quartz, glass, alumina, zirconia, and the like. The alumina is used as a low-cost ceramic raw material with wide sources, has the limitations of high brittleness and poor ductility in performance, and is used for producing grinding media, so that the product is easy to break in a high-energy grinding machine running at high speed; the zirconia is used as a ceramic raw material with better toughness, and can play a good toughening effect on the alumina material after being added.
Chinese patent publication No. CN101143783A discloses a zirconia toughened mullite ceramic material and a preparation method thereof, which adopts zirconium silicate and alpha-phase alumina as a matrix, applies modern toughening and strengthening technology, adds yttria, magnesia, calcium oxide and titanium oxide as mineralizers, and adds mullite as seed crystal. Compared with the alumina ceramic material, the invention has the advantages of high strength, high toughness, high wear resistance, simple production process, greatly reduced sintering temperature and energy saving and consumption reduction. The technical scheme discloses zirconium silicate and aluminum oxide and discloses yttrium oxide, magnesium oxide, calcium oxide and titanium oxide as mineralizers, wherein zirconium oxide is decomposed and toughened by adopting an in-situ reaction method, the zirconium silicate is low in decomposition efficiency under a low-temperature condition, silicon oxide generated by decomposition exists in a free state and mainly exists in a crystal phase form such as cristobalite and the like in the material, the free silicon dioxide is low in strength and poor in toughness, and expansion can occur due to crystal phase transformation during high-speed friction heating, so that the spherical medium is crushed, the structural stability is poor, and the toughness and the crushing resistance are reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-strength in-situ toughened alumina grinding ball for mineral deep processing, which is prepared by introducing zirconium dioxide through low-cost zirconium silicate and completely removing free silicon oxide generated by decomposition by adding a small amount of nano alumina to improve the overall toughness and crushing resistance of the material.
In order to realize the purpose of the invention, the following technical scheme is provided: a high-strength in-situ toughening alumina grinding ball for mineral deep processing comprises the following raw material powder in percentage by mass: matrix material: 60% -85% of aluminum oxide and 5% -25% of zirconium silicate; the method is characterized in that a sintering aid is added: 1 to 5 percent of zirconium oxide, 0.5 to 3 percent of yttrium oxide, 0.5 to 5 percent of calcium carbonate, 0.5 to 5 percent of magnesium carbonate and 0.5 to 5 percent of potassium carbonate; an inducer: 1 to 5 percent of nano alumina.
In order to achieve the object of the invention, the preparation method of the high-strength in-situ toughened alumina grinding ball for mineral deep processing according to claim 1 is characterized by comprising the following steps: mixing a matrix material: 60% -85% of aluminum oxide and 5% -25% of zirconium silicate; the method is characterized in that a sintering aid is added: 1 to 5 percent of zirconium oxide, 0.5 to 3 percent of yttrium oxide, 0.5 to 5 percent of calcium carbonate, 0.5 to 5 percent of magnesium carbonate and 0.5 to 5 percent of potassium carbonate; an inducer: mixing 1-5% of nano-alumina raw material powder, adding water, mixing the materials by a ball mill, grinding the materials by a stripping machine to obtain slurry meeting the requirement, spray-drying the slurry to obtain raw material powder, and forming the raw material powder by a ball rolling machine to obtain a biscuit ball; sintering the biscuit ball to obtain the compact high-strength high-wear-resistance toughened alumina ball.
Preferably, the sintering process is characterized by 100C/min heating to 10000C, then 2/min0C raising the temperature to the sintering temperature of 1450-0And C, preserving the temperature for 3-5 hours, and then naturally cooling to room temperature.
Preferably, the raw material powder: water: the proportion of the grinding balls is as follows: 1: 1.5: 3.
preferably, the diameter of the biscuit ball is 1-2 mm.
Preferably, the prepared toughened alumina grinding ball has the density of 3.8-4.0g/cm3The Vickers hardness is 1200-1350Gpa, and the fracture toughness is 2.8-3.8 MPa1/2The crushing strength is 1800-2000N, the self-abrasion is 1-2 g/hr.kg, and the belt material abrasion is 1-2 g/hr.kg.
The technical key points of the invention are as follows: industrial alumina and zirconium silicate are used as matrix materials, and zirconium oxide is generated through in-situ decomposition of zirconium silicate at medium and low temperature to toughen the alumina material. By introducing a special auxiliary agent and a nano alumina inducer with uniform high dispersion and utilizing the nano effect of high activity, a silicon-oxygen tetrahedral group in zirconium silicate begins to be captured at a lower temperature to induce the decomposition of the zirconium silicate and the formation of a mullite phase, firstly, the decomposition temperature of the zirconium silicate is reduced to achieve the purpose of the decomposition of the zirconium silicate at the medium and low temperature, secondly, a silicon oxide phase is reacted once being formed, the residue of a free silicon dioxide phase is avoided, and a new phase formed by the nano inducer and silicon oxide is uniformly distributed among main phase grains to form a stable structure, thereby achieving the aim of rapidly decomposing the zirconium oxide in situ at the low temperature to toughen the aluminum oxide.
The invention has the beneficial effects that: the invention has the advantages of low cost of raw materials, simple manufacturing process, realization of in-situ decomposition of zirconium silicate under the condition of medium and low temperature, avoidance of residue of free silicon dioxide phase, stable structure, obvious toughening effect and suitability for industrial application.
Detailed description of the invention
Example 1:
60 percent of aluminum oxide, 25 percent of zirconium silicate, 3 percent of yttrium oxide, 5 percent of nano aluminum oxide, 0.5 percent of calcium carbonate, 5 percent of potassium carbonate, 1 percent of zirconium oxide and 0.5 percent of magnesium carbonate.
Mixing the raw material powder in proportion, adding water and grinding balls, wherein the raw material powder comprises the following components in percentage by weight: water: the milling ball ratio was (1: 1.5: 3). Ball milling is carried out for 6 hours to obtain evenly mixed slurry, then a stripping machine is used for grinding for 3 hours to obtain slurry meeting the requirements, and spray drying is carried out to obtain raw material powder. And (3) spraying the raw material powder and water into a ball rolling machine, and forming by the ball rolling machine to obtain biscuit balls with the diameter of about 2 mm. And sintering the biscuit balls to obtain the zirconium silicate balls. The sintering process is as follows, 100C/min heating to 10000C, then 20C/min heating to sintering temperature 14500And C, keeping the temperature for 3 hours, and then naturally cooling to room temperature. The prepared toughened alumina grinding ball has the density of 3.9g/cm3The Vickers hardness is 1250Gpa, and the fracture toughness is 3.2 MPa1/2The crushing strength was 1800N, the self-abrasion was 1.0 g/hr.kg, and the belt abrasion was 1.2 g/hr.kg.
Example 2:
70 percent of alumina, 17 percent of zirconium silicate, 2 percent of yttrium oxide, 2 percent of nano alumina, 5 percent of calcium carbonate, 0.5 percent of potassium carbonate, 1.5 percent of zirconium oxide and 2 percent of magnesium carbonate.
Mixing the raw material powder in proportion, adding water and grinding balls, wherein the raw material powder comprises the following components in percentage by weight: water: the milling ball ratio was (1: 1.5: 3). Ball milling is carried out for 6 hours to obtain evenly mixed slurry, then a stripping machine is used for grinding for 3 hours to obtain slurry meeting the requirements, and spray drying is carried out to obtain raw material powder. And (3) spraying the raw material powder and water into a ball rolling machine, and forming by the ball rolling machine to obtain biscuit balls with the diameter of about 2 mm. And sintering the biscuit balls to obtain the zirconium silicate balls. The sintering process is as follows, 100C/min heating to 10000C, then 20C/min heating to sintering temperature 15000And C, keeping the temperature for 4 hours, and then naturally cooling to room temperature. The prepared zirconium silicate grinding ball has the density of 3.7g/cm3Vickers hardness of 1200Gpa and fracture toughness of 3.0 MPa1/2The crushing strength was 1600N, the self-abrasion was 1.2 g/hr.kg, and the belt abrasion was 1.3 g/hr.kg.
Examples 3 to 6 are shown in the following tables:
| alumina oxide | Zirconium silicate | Yttria | Nano alumina | Calcium carbonate | Potassium carbonate | Zirconium oxide | Magnesium carbonate | |
| Example 3 | 65 | 20 | 2 | 2.5 | 1.5 | 2 | 5 | 2 |
| Example 4 | 77 | 15 | 1.5 | 1.5 | 1 | 0.5 | 1 | 2.5 |
| Example 5 | 80 | 10 | 1 | 3 | 2 | 0.5 | 0.5 | 3 |
| Example 6 | 85 | 5 | 0.5 | 1 | 1 | 1 | 1.5 | 5 |
Claims (4)
1. A preparation method of a high-strength in-situ toughening alumina grinding ball for mineral deep processing comprises the following steps: the raw material powder comprises the following components in percentage by mass: matrix material: 60% -85% of aluminum oxide and 5% -25% of zirconium silicate; the method is characterized in that a sintering aid is added: 1 to 5 percent of zirconium oxide, 0.5 to 3 percent of yttrium oxide, 0.5 to 5 percent of calcium carbonate, 0.5 to 5 percent of magnesium carbonate and 0.5 to 5 percent of potassium carbonate; an inducer: mixing 1-5% of nano-alumina raw material powder, adding water, mixing the materials by a ball mill, grinding the materials by a stripping machine to obtain slurry meeting the requirement, spray-drying the slurry to obtain raw material powder, and forming the raw material powder by a ball rolling machine to obtain a biscuit ball; sintering the biscuit balls to obtain compact high-strength high-wear-resistance toughened alumina balls; the sintering process is characterized in that the temperature is raised to 1000 ℃ at the speed of 10 ℃/min and then 2/min0C, raising the temperature to 1450 and 1500 ℃ of sintering temperature, preserving the temperature for 3-5 hours, and then naturally cooling to room temperature.
2. The preparation method of the high-strength in-situ toughening alumina grinding ball for mineral deep processing according to claim 1, characterized in that the raw material powder: water: the proportion of the grinding balls is as follows: 1: 1.5: 3.
3. the method for preparing the high-strength in-situ toughening alumina grinding ball for mineral deep processing according to claim 1, wherein the diameter of the biscuit ball is 1-2 mm.
4. The high-strength in-situ toughening oxygen for mineral deep processing according to claim 1The preparation method of the aluminum oxide grinding ball is characterized in that the prepared toughened aluminum oxide grinding ball has the density of 3.8-4.0g/cm3The Vickers hardness is 1200-1350Gpa, and the fracture toughness is 2.8-3.8 MPa1/2The crushing strength is 1800-2000N, the self-abrasion is 1-2 g/hr.kg, and the belt material abrasion is 1-2 g/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 |
| 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 |
| 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 |
| 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 |
| CN114538920B (en) * | 2022-03-17 | 2023-02-03 | 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 |
| CN115340369B (en) * | 2022-10-18 | 2023-01-24 | 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 |
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