CN113735571A - Grinding medium and preparation method thereof - Google Patents
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- CN113735571A CN113735571A CN202111076231.7A CN202111076231A CN113735571A CN 113735571 A CN113735571 A CN 113735571A CN 202111076231 A CN202111076231 A CN 202111076231A CN 113735571 A CN113735571 A CN 113735571A
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Abstract
The invention discloses a grinding medium which comprises the following raw materials in percentage by weight: a first raw material group: 90-95% of alumina powder, 0.5-2.0% of calcined talc, 1.0-3.0% of dolomite, 3.0-5.5% of Suzhou soil and 0.3-0.8% of yttrium oxide; a second raw material group: 0.2-1.0% of plasticizer and 0.2-1.0% of dispersant, and the invention also discloses a preparation method of the grinding medium. According to the invention, the content of alumina in the grinding medium is increased, so that the liquid phase amount in the sintering process is reduced, the finally prepared grinding medium has low vitrification degree and larger crystal boundary energy, large cracks are difficult to generate in the impact process, and the impact resistance of the grinding medium is greatly increased, so that the grinding medium is suitable for severe dry grinding environment.
Description
Technical Field
The invention belongs to the technical field of grinding materials, and particularly relates to a grinding medium and a preparation method thereof.
Background
The microcrystalline alumina grinding medium has excellent performances of corrosion resistance, high grinding efficiency, good quality and the like, is widely applied to industries such as ore dressing, ceramics, electronic materials, magnetic materials, coatings, paints and the like, has excellent grinding effect when being applied to the wet grinding industry, but has certain limitation on the grinding effect in the dry grinding industry, and is easy to generate the phenomenon of ceramic collapse, mainly because in the wet grinding environment, the grinding medium is subjected to the resistance of slurry during grinding, which is equivalent to the increase of buffer in the collision process, and the temperature of the slurry is generally lower and is less than eighty-nine degrees, so that the environment for using the product is better, and the microcrystalline alumina grinding medium can completely perform grinding work. However, in the dry grinding environment, solid particles are generally ground, the uniformity of materials is poor, and more balls are hard to touch and harden in the grinding process, so that the buffer in the dry grinding environment is not sufficient, most dry grinding has low grinding efficiency, the heat production is large, and the temperature is difficult to reduce, so that the use environment is much worse than the wet grinding, and the peeling phenomenon of grinding media, namely the phenomenon of ceramic breaking, is easy to occur.
Thus, there is a need for an impact resistant alumina grinding media that meets the needs of a dry milling environment.
Disclosure of Invention
In order to solve the defects of the prior art, the invention discloses an impact-resistant alumina grinding medium, which adopts the following technical scheme:
a grinding medium comprises the following raw materials in percentage by weight:
a first raw material group: 90 to 95% of alumina powder, for example, 90%, 92%, 95%;
0.5 to 2.0% of calcined talc, for example, may be 0.5%, 1.0%, 2.0%;
1.0 to 3.0% of dolomite, for example, 1.0%, 2.0%, 3.0%;
2.0 to 5.5% of Suzhou soil, for example, 2.0%, 3.5%, 5.5%;
0.3 to 0.8% of yttrium oxide, for example, 0.3%, 0.5%, 0.8%;
a second raw material group: 0.2 to 1.0% of a plasticizer, for example, 0.2%, 0.5%, 1.0%;
and 0.2 to 1.0% of a dispersant, for example, 0.2%, 0.5%, 1.0%.
Further, the first raw material group further includes 0.3 to 0.8% of lanthanum oxide, for example, 0.3%, 0.5%, 0.8% and 0.5 to 1.5% of barium carbonate may be selected, for example, 0.5%, 1.0%, 1.5% may be selected.
Further, the sodium content in the alumina powder is lower than 0.15%.
Further, the plasticizer is polyvinyl alcohol and/or methyl cellulose.
Further, the dispersing agent is polyacrylate and/or sodium tripolyphosphate.
The invention also discloses a preparation method of any one of the grinding media, which comprises the following steps:
adding the first raw material group into a grinding machine for grinding, adding the second raw material group, and uniformly mixing to obtain mixed slurry;
and drying the mixed slurry to prepare powder to obtain granulated powder, carrying out isostatic pressing on the granulated powder to obtain a green body, and sintering the green body at a high temperature to finally obtain the grinding medium.
Furthermore, the time of the grinding process is 24-36 h, for example, 24h, 28h, 32h, and 36 h.
Furthermore, the equipment adopted in the drying and pulverizing process is a centrifugal spray granulation tower.
Further, the rotating speed of a centrifugal disc of the centrifugal spray granulation tower is 800-12000 r/min, such as 800r/min, 5000r/min, 1000r/min and 12000r/min, the inlet temperature of a hearth is 300-500 ℃, such as 300 ℃, 400 ℃ and 500 ℃, and the outlet temperature is 80-120 ℃, such as 80 ℃, 100 ℃ and 120 ℃.
Further, the equipment used for high-temperature sintering is a tunnel kiln, the temperature in the sintering process is 1410-1550 ℃, for example, 1410 ℃, 1500 ℃ and 1550 ℃, and the heat preservation time is 4.0-5.0 h, for example, 4.0h, 4.5h and 5.0 h. And the heat preservation time in the prior art is generally more than 6.5 h.
By adopting the technical scheme, the invention has the beneficial effects that:
1) according to the invention, the content of alumina in the grinding medium is increased, the liquid phase amount in the sintering process is reduced, the final prepared grinding medium has low vitrification degree, abnormal growth of crystal grains is reduced, the probability of occurrence of lattice defects is reduced, and the condition of transgranular fracture is reduced, so that higher crystal boundary energy can be maintained, large cracks are difficult to generate in the impact process, the impact resistance of the grinding medium is greatly increased, and the grinding medium is suitable for a severe dry grinding environment.
2) According to the invention, lanthanum oxide is added into the grinding medium, so that the phenomenon of abnormal growth of alumina grains caused by the increase of the content of alumina is overcome, and the impact resistance of the grinding medium is further ensured.
Drawings
FIG. 1 is a scanning electron micrograph (4 μm) of a prior art grinding medium
FIG. 2 is a scanning electron micrograph (10 μm) of a prior art grinding medium
FIG. 3 is a scanning electron micrograph (4 μm) of the grinding medium of the present invention
FIG. 4 is a scanning electron micrograph (10 μm) of the grinding medium of the present invention
FIG. 5 is a scanning electron microscope image of the first embodiment of the invention
FIG. 6 is a scanning electron microscope image of a second embodiment of the present invention
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a grinding medium which comprises the following raw materials in percentage by weight: a first raw material group: 90-95% of alumina powder, 0.5-2% of calcined talc, 1-3% of dolomite, 1.5-5.5% of kaolin and 0.3-0.8% of yttrium oxide; a second raw material group: 0.2-1.0% of plasticizer and 0.2-1.0% of dispersing agent, wherein the plasticizer can be polyvinyl alcohol and/or methyl cellulose, and the dispersing agent can be polyacrylate and/or sodium tripolyphosphate.
The content of alumina powder in a grinding medium in the prior art is about 80%, in order to increase the impact resistance of the alumina grinding medium, the method adopted in the prior art is to reduce the content of alumina in the grinding medium and simultaneously increase the content of a toughening agent, the toughening agent usually selected is zirconia, the impact resistance of the grinding medium can be improved to a certain degree by increasing the content of zirconia, but the zirconia is expensive, and the production cost is greatly increased.
The invention can obviously improve the impact resistance of the finally prepared grinding medium by increasing the content of the alumina, namely increasing the content of the alumina to 90-95 percent, mainly because the grinding medium needs to be sintered at a high temperature of more than one thousand degrees during preparation, in the high-temperature sintering process, the added fluxing agents, such as components of calcined talc, dolomite, Suzhou soil and the like, can be melted to generate a liquid phase, the vitrification degree is higher as the liquid phase is more, and the finally prepared grinding medium finished product is easy to generate larger cracks in the impact process, so that the peeling phenomenon is generated, which is also one reason that the porcelain collapse phenomenon is easy to generate in the dry grinding process. The aluminum oxide can not be melted at the sintering temperature of more than one thousand degrees, so the invention reduces the liquid phase amount in the sintering process by increasing the proportion of the aluminum oxide in the grinding medium, the finally prepared grinding medium has low vitrification degree, larger grain boundary energy, difficult generation of large cracks in the impact process and better impact resistance.
Fig. 1 to 4 are electron microscope images of two kinds of alumina grinding media, wherein fig. 1 and 2 are scanning electron microscope images of a grinding medium with an alumina content of 80% in the prior art (fig. 1 is a photograph under 4 micrometers, fig. 2 is a photograph under 10 micrometers), fig. 3 and 4 are scanning electron microscope images of a grinding medium with an alumina content of 94% in the present invention (fig. 3 is a photograph under 4 micrometers, fig. 4 is a photograph under 10 micrometers), and as can be seen by comparing fig. 1, 2, 3 and 4, the crystal grain growth in the cross section of fig. 1 and 2 is disordered, the crystal grain size is large, the number of lattice defects is large, the fracture is transgranular fracture, the cross section is flat and has no resistance, and the product belongs to a product with more obvious brittleness, and the impact resistance is poor; the crystal grains in the cross sections of the images 3 and 4 are uniform, the isotropy of the growing part of the crystal grains is obvious, and the fracture surfaces are fractured along the crystal, so that higher fracture energy is needed during cracking, the crystal lattice defects are few, a small amount of microcracks exist, the bridge chain effect is achieved, the cracks are changed in direction, the fracture potential energy is increased, and the impact resistance is improved.
Therefore, the invention greatly increases the impact resistance of the grinding medium by increasing the content of the alumina in the grinding medium, so that the grinding medium is suitable for a severe dry grinding environment, and simultaneously, zirconia is not required to be added as a toughening agent, thereby greatly reducing the production cost.
In a preferred embodiment of the present invention, the first raw material set further comprises 0.3-0.8% of lanthanum oxide and 0.5-1.5% of barium carbonate.
The grinding medium has wide application and large consumption, so a tunnel kiln is usually selected for high-temperature sintering during preparation to meet the requirements of continuous and mass production, when the high-temperature sintering is carried out by using the tunnel kiln, the sintering temperature needs to be controlled within 1550 ℃, which is determined by the structural property of the tunnel kiln, the sintering temperature of the alumina is higher, and the sintering temperature can be increased by 15-20 ℃ when the content of the alumina is increased by 1 percent, therefore, after the content of the alumina is increased, the sintering temperature becomes a difficult point in the preparation process of the impact-resistant grinding medium, the method of reducing the sintering temperature and prolonging the heat preservation time is generally adopted in the prior art to overcome the problem, however, the extension of the heat preservation time brings a new problem, and experiments show that the extension of the heat preservation time can cause abnormal growth of crystal grains of the prepared grinding medium and more defects.
The inventor discovers through a large amount of experiments, through adding lanthanum oxide in the preparation process, can improve the unusual big phenomenon of crystalline grain, but because lanthanum oxide when being heated inhomogeneous, can influence the effect of improving the crystalline grain, discover through the experiment, add barium carbonate in the lanthanum oxide reagent, in the high temperature sintering process, barium carbonate parcel is around lanthanum oxide, because barium carbonate's high thermal conductivity, can be so that the lanthanum oxide that is surrounded is heated evenly, can not ftracture, and then guarantee that lanthanum oxide suppresses the unusual effect of growing up of alumina crystalline grain. Meanwhile, experiments show that the addition of barium carbonate can shorten the heat preservation time, namely after the barium carbonate is added, the sintering requirement can be met in a shorter heat preservation time, the heat preservation time is shortened, and the abnormal growth of crystal grains is inhibited to a certain extent.
Namely, the lanthanum oxide and barium carbonate are combined to reduce the probability of crystal grain defects caused by prolonging the heat preservation time, and further ensure the impact resistance of the grinding medium.
The inventors prepared comparative example 1 and example 1 by selecting raw materials within the scope of the present disclosure, and the comparative example 1 and example 1 were different only in that: the barium carbonate is additionally added in 1 percent in example 1, the heat preservation time is shortened to 4.5h, the barium carbonate is not added in comparative example 1, the heat preservation time is 6.5h, other preparation conditions of comparative example 1 and example 1 are the same, after tests, the volume density of comparative example 1 is about 3.64, the volume density of example 1 is about 3.63, and the difference between the two is small, which shows that the heat preservation time is shortened after the barium carbonate is added, the required sintering volume density can be achieved, the sintering time is shortened, and the abnormal growth of crystal grains is inhibited to a certain extent.
As shown in fig. 5 and 6, fig. 5 and 6 are both electron microscope scanning images of the grinding medium prepared by high-temperature sintering in a tunnel kiln after the content of alumina is increased to 94.5%, fig. 5 is an electron microscope scanning image of the grinding medium prepared without adding lanthanum oxide and barium carbonate and with the heat preservation time of 6.5h, and fig. 6 is an electron microscope scanning image of the grinding medium prepared with lanthanum oxide and barium carbonate and with the heat preservation time of 4.5 h.
In one embodiment of the invention, the sodium content of the alumina powder is less than 0.15%, and sodium ions are destructive to the alumina crystals during the preparation process, and this interference can be avoided by selecting a low sodium alumina powder.
Examples 2 and 3 disclose methods of making grinding media of the present invention, wherein the specific process of making example 2 is:
93% of alumina powder, 0.5% of calcined talc, 1.0% of dolomite, 2.5% of kaolin, 0.5% of yttrium oxide, 0.5% of lanthanum oxide and 1.0% of barium carbonate. Adding the mixture into a grinding machine for grinding for 30 hours, adding 0.5% of plasticizer and 0.5% of dispersant, and uniformly mixing to obtain mixed slurry; drying the mixed slurry to prepare powder, obtaining granulated powder, performing isostatic pressing on the granulated powder by using a bag-type rubber mold (a binder can be added according to needs in the isostatic pressing process) to obtain a blank, and sintering the blank at a high temperature to finally obtain the grinding medium.
Wherein, the equipment adopted in the drying and pulverizing process can be a centrifugal spray granulation tower, a 2500 type centrifugal spray granulation tower is selected, the rotating speed of a centrifugal disc is 8000r/min, the inlet temperature of a hearth is 400 ℃, and the outlet temperature is 100 ℃.
The equipment used for high-temperature sintering is a ninety-meter tunnel kiln, the temperature in the sintering process is 1510 ℃, and the heat preservation time is 5.0 h.
The specific preparation process of example 3 is:
95% of alumina powder, 0.5% of calcined talc, 1.0% of dolomite, 2.0% of kaolin, 0.3% of yttrium oxide, 0.3% of lanthanum oxide and 0.5% of barium carbonate. Adding the mixture into a grinding machine for grinding for 36 hours, adding 0.2% of plasticizer and 0.2% of dispersant, and uniformly mixing to obtain mixed slurry; drying the mixed slurry to prepare powder, obtaining granulated powder, performing isostatic pressing on the granulated powder by using a bag-type rubber mold (a binder can be added according to needs in the isostatic pressing process) to obtain a blank, and sintering the blank at a high temperature to finally obtain the grinding medium.
The equipment used in the drying and pulverizing process can be a centrifugal spray granulation tower, for example, a 2500-type centrifugal spray granulation tower, wherein the rotation speed of a centrifugal disc of the centrifugal spray granulation tower is 12000r/min, the inlet temperature of a hearth is 500 ℃, and the outlet temperature is 120 ℃.
The equipment used for high-temperature sintering is a tunnel kiln, the temperature in the sintering process is 1550 ℃, and the heat preservation time is 4.5 h.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still modify the technical solutions described in the foregoing embodiments, or may equally substitute some or all of the technical features; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. A grinding media characterized by: comprises the following raw materials in percentage by weight:
a first raw material group: 90-95% of alumina powder, 0.5-2.0% of calcined talc, 1.0-3.0% of dolomite, 2.0-5.5% of Suzhou soil and 0.3-0.8% of yttrium oxide;
a second raw material group: 0.2 to 1.0 percent of plasticizer and 0.2 to 1.0 percent of dispersant.
2. The grinding media of claim 1, wherein: the first raw material group further comprises 0.3-0.8% of lanthanum oxide and 0.5-1.5% of barium carbonate.
3. The grinding media of claim 1, wherein: the sodium content in the alumina powder is lower than 0.15%.
4. Grinding media according to claim 1, wherein the plasticizer is polyvinyl alcohol and/or methyl cellulose.
5. Grinding media according to claim 1, wherein the dispersant is polyacrylate and/or sodium tripolyphosphate.
6. A method of making the grinding media of any of claims 1 to 5, wherein: the method comprises the following steps:
adding the first raw material group into a grinding machine for grinding, adding the second raw material group, and uniformly mixing to obtain mixed slurry;
and drying the mixed slurry to prepare powder to obtain granulated powder, carrying out isostatic pressing on the granulated powder to obtain a green body, and sintering the green body at a high temperature to finally obtain the grinding medium.
7. The preparation method according to claim 6, wherein the time of the grinding process is 24-36 hours.
8. The method of claim 6, wherein: the equipment adopted in the drying and pulverizing process is a centrifugal spray granulation tower.
9. The method of claim 8, wherein: the rotating speed of a centrifugal disc of the centrifugal spray granulation tower is 800-12000 r/min, the inlet temperature of a hearth is 300-500 ℃, and the outlet temperature is 80-120 ℃.
10. The method of claim 6, wherein: the equipment used for high-temperature sintering is a tunnel kiln, the temperature in the sintering process is 1410-1550 ℃, and the heat preservation time is 4.0-5.0 h.
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