CN105367054A - Preparation method for gel-casting system-based zirconium dioxide ball-milling medium - Google Patents
Preparation method for gel-casting system-based zirconium dioxide ball-milling medium Download PDFInfo
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Abstract
The invention relates to a preparation method for a gel-casting system-based zirconium dioxide ball-milling medium. The preparation method comprises the steps of: providing yttria-stabilized tetragonal phase zirconium oxide powder, deionized water, a crosslinking agent, a monomer, a dispersant, an initiator, a catalyst and an oil phase forming agent; stirring and mixing the monomer, the crosslinking agent, the dispersant and the deionized water to obtain a pre-prepared mixed liquid; ball-milling the pre-prepared mixed liquid and the yttria-stabilized tetragonal phase zirconium oxide powder to obtain pre-prepared slurry; ball-milling the pre-prepared slurry and the initiator to obtain zirconium oxide cermamic slurry; separately spraying out the zirconium oxide cermamic slurry and the catalyst in the form of liquid drops by adopting a spraying process and spraying the mixture into the oil phase forming agent; filtering, washing and drying the mixture to obtain a prefabricated zirconium dioxide ball-milled medium green body and washing the green body by using carbon tetrachloride; and sintering the prefabricated zirconium dioxide ball-milled medium green body to obtain a sub-millimeter-scale zirconium dioxide ball-milled medium. The preparation method has the advantages of being relatively simple in preparation process and relatively low in cost.
Description
Technical field
The present invention relates to ball-milling medium preparing technical field, particularly relate to a kind of preparation method of the zirconium dioxide ball-milling medium based on gel injection system.
Background technology
At present, ball mill, as the major equipment in the operation of mineral aggregate comminution, is widely applied in the mineral aggregate comminution process of numerous industries such as metallurgy, building materials, chemical industry, along with it is since appearance in 1893, so far the history of existing more than 100 year, remarkable contribution has been made in the development of civilization for the mankind.
Wherein, grinding ballstone is the ball or cylindrical object that roll in ball mill, is commonly called as ball-milling medium.Especially in ceramic production industry, the mainly Ceramic Balls grinding media used, zirconia ball grinding media is with numerous outstanding advantages such as high strength, high rigidity, excellent wear resistance and erosion resistances, show one's talent in many series ceramic ball-milling mediums, and extensively by the favor of ceramic industry, prepare in industry at zirconia ceramics, apply especially extensive.
But along with the progress of science and technology and the fast development of periphery industry, traditional particle diameter is greater than the zirconia ball grinding media of 1 millimeter (mm), and namely zirconia ceramics ball can not meet the demand of the ultra-fine ball milling of industry.
For the problems referred to above, sight focuses in other zirconia ceramics ball of submillimeter level by scientific researcher gradually, especially the fast development of the industry of ultra-fine ball milling is needed along with coating and ink etc., it is more urgent to the demand of other zirconia ceramics ball of submillimeter level, and have developed the zirconia ceramics ball of 0.3mm rank thus, and its consumption there has also been and significantly increases.But the zirconia ceramics ball preparing the performances such as wear resistance preferably 0.1mm ~ 0.3mm rank still becomes present stage problem demanding prompt solution.
The preparation method of other zirconia ceramics ball of traditional submillimeter level mainly contains mould pressing, isostatic pressing method, atomization and spray granulation etc., but existing preparation method still has relative density difference and the low defect of physical strength, and above-mentioned preparation method's ubiquity complex process, the problem that cost is higher.
Summary of the invention
Based on this, be necessary to provide the preparation method of the zirconium dioxide ball-milling medium based on gel injection system that a kind of technique is comparatively simple, cost is lower, can prepare other zirconium dioxide ball-milling medium of submillimeter level.
Based on a preparation method for the zirconium dioxide ball-milling medium of gel injection system, comprise the steps:
Yttrium is provided to stablize tetragonal phase zirconium oxide powder, deionized water, linking agent, monomer, dispersion agent, initiator, facilitate agent and oil phase forming agent;
Described monomer, described linking agent, described dispersion agent and described deionized water and stirring are mixed, obtains prewired mixed solution;
Described prewired mixed solution and described yttrium are stablized after tetragonal phase zirconium oxide powder mixes, be added to after carrying out ball milling operation in ball grinder, obtain prewired slurry;
After described prewired slurry is mixed with described initiator, be added to after carrying out ball milling operation in ball grinder, obtain zirconia ceramic slurry;
Adopt spray art described zirconia ceramic slurry and described catalyzer to be sprayed with the form of drop respectively, and after making both droplets mixings, spray into in described oil phase forming agent simultaneously;
By filtering, wash and after drying, obtaining prefabricated zirconium dioxide ball-milling medium green compact, wherein, tetracol phenixin is adopted to carry out described washing operation;
After described prefabricated zirconium dioxide ball-milling medium green sintering, obtain the described zirconium dioxide ball-milling medium of submillimeter level.
Wherein in an embodiment, described dispersion agent comprises at least one in ammonium citrate and ammonium polyacrylate.
Wherein in an embodiment, described dispersion agent is ammonium citrate.
Wherein in an embodiment, described tetracol phenixin is adopted to carry out repeatedly described washing operation.
Wherein in an embodiment, described filter operation is vacuum filtration.
Wherein in an embodiment, the median particle diameter of the described zirconium dioxide ball-milling medium of submillimeter level is 0.1mm ~ 0.3mm.
Wherein in an embodiment, the time that described drying operation continues is 18 hours ~ 24 hours.
The preparation method of the above-mentioned zirconium dioxide ball-milling medium based on gel injection system utilizes the reactive force between two-phase interface can obtain the described zirconium dioxide ball-milling medium of submillimeter level, relative to traditional preparation method, there is the simpler and lower-cost advantage of preparation technology.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the zirconium dioxide ball-milling medium based on gel injection system of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
As shown in Figure 1, the preparation method of the zirconium dioxide ball-milling medium based on gel injection system of an embodiment, comprises the steps:
S110: provide yttrium to stablize tetragonal phase zirconium oxide powder, deionized water, linking agent, monomer, dispersion agent, initiator, facilitate agent and oil phase forming agent.
In one embodiment, the median particle diameter of described stable tetragonal phase zirconium oxide powder is 1.9 μm ~ 2.5 μm, adopt the stable tetragonal phase zirconium oxide powder of above-mentioned median particle diameter can prepare dispersion evenly zirconia ceramic slurry, and the shape of the follow-up zirconium dioxide ball-milling medium prepared can be made more well-balanced, and namely its ball-like structure is more even.Preferably, the median particle diameter of described stable tetragonal phase zirconium oxide powder is 2.1 μm.
S120: described monomer, described linking agent, described dispersion agent and described deionized water and stirring are mixed, obtains prewired mixed solution.
In one embodiment, each component of following mass parts is adopted to be uniformly mixed, obtain described prewired mixed solution: described monomer 1 part ~ 1.5 parts, described linking agent 0.05 part ~ 0.1 part and described dispersion agent 15 parts ~ 20 parts, and appropriate deionized water, wherein, the consumption of described deionized water can guarantee that described prewired mixed solution has suitable viscosity.
In one embodiment, described monomer is acrylamide, and described linking agent is N, N
,-methylene-bisacrylamide, described initiator is ammonium persulphate, described in facilitate agent be Tetramethyl Ethylene Diamine, above-mentioned four are used for making zirconium white idiosome carry out solidify in place process, namely gelling system is formed, to realize Gel-casting process, in the present embodiment, aqueous gel system is formed, to realize Gel-casting process, so, can avoid with an organic solvent, reduce the volatilization of organic solvent.
In one embodiment, described dispersion agent comprises at least one in ammonium citrate and ammonium polyacrylate, and preferably, described dispersion agent is ammonium citrate.
S130: described prewired mixed solution and described yttrium are stablized after tetragonal phase zirconium oxide powder mixes, be added to after carrying out ball milling operation in ball grinder, obtain prewired slurry.
Mix by described prewired mixed solution and described yttrium are stablized tetragonal phase zirconium oxide powder, and utilize the effect of the described dispersion agent in described prewired mixed solution, yttrium can be made to stablize tetragonal phase zirconium oxide powder to be more uniformly dispersed in described prewired mixed solution, namely described dispersion agent is passed through as dispersion medium, described yttrium can be made to stablize tetragonal phase zirconium oxide powder and described monomer and described linking agent mixedly more even, and form more stable suspension system, namely described yttrium is stablized tetragonal phase zirconium oxide powder and is existed with the form of suspended particles, be beneficial to follow-up solidify in place process, thus it is even to obtain particle dispersion, the slurry of good fluidity and high solidification content.
Be appreciated that, utilize the prewired slurry of high solid loading and good fluidity, the zirconium dioxide ball-milling medium prepared is when sintering, the situation that can reduce strain cracking occurs, namely can realize the sintering effect of near net-shape, namely reduce shrinking percentage, and overall mechanical properties be stronger, and for example, wear resistance, uniformity coefficient, erosion resistance are all stronger.
In one embodiment, described ball milling operation carries out on planetary ball mill; And for example, described ball grinder is nylon tank; And for example, described ball milling operation adopts zirconia ball as ball-milling medium; And for example, described zirconia ball and described yttrium stablize the mass ratio of tetragonal phase zirconium oxide powder is 1:(4 ~ 6); And for example, the diameter of described zirconia ball is 3mm ~ 5mm; And for example, the Ball-milling Time of described ball milling operation is 4 hours ~ 5 hours; And for example, the rotating speed of described planetary ball mill is 380r/min ~ 420r/min, like this, be conducive to obtaining the better and particle diameter of dispersion effect evenly prewired slurry.
It should be noted that, ammonium citrate as dispersion agent is a kind of small molecule anionic type dispersion agent, main dispersion mechanism is that DLVO (i.e. electrostatic stabilization) is theoretical, when the addition of ammonium citrate is lower, adsorption concentration on its particle surface in described this suspension system of prewired slurry is low, namely to stablize the adsorption concentration of tetragonal phase zirconium oxide powder low for the yttrium of its surface adsorption, be unfavorable for that yttrium is stablized tetragonal phase zirconium oxide powder and is present in described prewired slurry with suspension system, now, described ammonium citrate is random arrangement, predominant intermolecular forces between particle appoints the electrostatic attraction shown as between non-adsorption particle, namely the yttrium do not adsorbed stablizes tetragonal phase zirconium oxide powder with the electrostatic attraction of self to realize dispersion effect, like this, dispersion effect extreme difference, so the viscosity of described prewired slurry is very big, rheological is poor, and particle dispersion is also even not.But, when the addition of ammonium citrate is too much, its particle surface in suspension system will produce multilayer absorption, and the positive-negative polarity of adjacent two layers is contrary, after both offset, yttrium is stablized between tetragonal phase zirconium oxide powder and can be disperseed in the mode of electrostatic attraction again, instead of is adsorbed on dispersant particle surface to disperse.The dispersed homogeneous degree of tetragonal phase zirconium oxide powder is stablized in order to improve yttrium, to reduce viscosity, thus raising rheological, such as, the mass ratio that described dispersion agent and described yttrium stablize tetragonal phase zirconium oxide powder is 1:(2 ~ 3), preferably, the mass ratio that described ammonium citrate and described yttrium stablize tetragonal phase zirconium oxide powder is 1:(2 ~ 3), preferably, the mass ratio that described ammonium citrate and described yttrium stablize tetragonal phase zirconium oxide powder be 1:2.5 like this, the viscosity of described prewired slurry can reach 9mPa
.below s, so, can improve the dispersed homogeneous degree that yttrium stablizes tetragonal phase zirconium oxide powder, to reduce viscosity, thus improves rheological.
S140: after described prewired slurry is mixed with described initiator, be added to after carrying out ball milling operation in ball grinder, obtain zirconia ceramic slurry.
The solid load of the zirconia ceramic slurry prepared by step 140 is 65% ~ 75%, and the viscosity of described zirconia ceramic slurry is 2mPa
.s ~ 8mPa
.s, like this, has the advantage of high solid loading, low viscosity and high rheological variation.
In one embodiment, the mass ratio of described monomer, described linking agent, described dispersion agent and described initiator is (1 ~ 1.5): (0.05 ~ 0.1): (15 ~ 20): (0.05 ~ 0.1).
Be appreciated that, because ball milling operation can produce a large amount of heats, make aqueous gel system can occur under the effect of described initiator liquid zirconia ceramic slurry shift to an earlier date gel forming solidification problem, in order to extend the storage life of described zirconia ceramic slurry, to guarantee carrying out smoothly of follow-up spray operation, and the carrying out of follow-up green compact normal gel solidification, such as, the mass ratio of described monomer and described initiator is (1 ~ 1.5): (0.05 ~ 0.1), preferably, the mass ratio of described monomer and described initiator is 1:0.1, like this, not only can guarantee carrying out smoothly of follow-up spray operation, namely the problem of gel solidification can not too fastly be there is, be beneficial to and extend the storage life, and, also can not be very few because of the consumption of described initiator, occur that green compact gel in situ solidifies abnormal problem.So, the storage life of described zirconia ceramic slurry can reach 1 hour ~ 1.5 hours, has enough surge time to carry out follow-up spray operation.
Further, the storage temperature of described zirconia ceramic slurry also has larger impact to the length of device shelf time, in order to extend the storage life of described zirconia ceramic slurry, to guarantee carrying out smoothly of follow-up spray operation, and the carrying out of follow-up green compact normal gel solidification, such as, after described ball milling operation, also cooling process is carried out to described zirconia ceramic slurry, with 2 DEG C/min, namely the lower the temperature rate of temperature fall of 2 degrees Celsius of per minute is cooled to 35 DEG C ~ 40 DEG C, like this, on the one hand, the phenomenon of the appearance instability of this suspension system of zirconia ceramic slurry temperature decrease can being avoided to bring with the rate of temperature fall of 2 DEG C/min, on the other hand, under the temperature condition of 35 DEG C ~ 40 DEG C, described zirconia ceramic slurry is preserved, not only can avoid described zirconia ceramic slurry under the effect of described initiator, occur the problem that premature gelation is solidified, and, the phenomenon of the appearance instability of this suspension system of zirconia ceramic slurry that too low temperature can also be avoided to bring.So, greatly the shelf time can be extended.
S150: adopt spray art described zirconia ceramic slurry and described catalyzer to be sprayed with the form of drop respectively, and after making both droplets mixings, spray into in described oil phase forming agent simultaneously.
Respectively described zirconia ceramic slurry and described catalyzer are sprayed with the form of drop by adopting spray art, namely two spraying equipment are adopted, as, specifically comprise the first spraying equipment and the second spraying equipment, described first spraying equipment sprays described zirconia ceramic slurry, and makes described zirconia ceramic slurry form drops, described second spraying equipment sprays described catalyzer, as, described catalyzer is Tetramethyl Ethylene Diamine, described second spraying equipment sprays described Tetramethyl Ethylene Diamine, and for example, described second spraying equipment sprays described Tetramethyl Ethylene Diamine solution, like this, described zirconia ceramic slurry drop and described Tetramethyl Ethylene Diamine solution droplets are aloft met and mix, spray into in oil phase forming agent together based on the inertia of self after both droplets mixings, as, described oil phase forming agent is whiteruss, spray into in described whiteruss after both droplets mixings, the zirconium dioxide ball-milling medium green compact of ball-like structure can be formed.
Here, again the moulding mechanism of above-mentioned zirconium dioxide ball-milling medium green compact is described, for multiphase system, have certain thickness area of space between the two-phase of close contact, this region is called interfacial layer or upper layer, and the thickness of wherein said interfacial layer is often thinner, it is only by the thickness of unit molecule city or several molecular layer, therefore, this interfacial layer can be similar to regards a face as, is commonly called as interface.Wherein, be in the molecule of phase boundary surface layer, as zirconia ceramic slurry is different from the stressing conditions being in molecule inner mutually via the gel particles formed after catalyst, the reactive force that molecule mutually receives surrounding molecular is symmetrical, can cancel out each other, make a concerted effort to be zero, and interfacial layer molecule, namely zirconia ceramic slurry is not only subject to the reactive force of phase interior molecules via the gel particles formed after catalyst, also be subject to another phase molecule simultaneously, the i.e. reactive force of whiteruss molecule, two kinds of reactive forces are not full symmetrics, can not repeal by implication, so interfacial layer molecule must be subject to the effect of the power in a direction, this be described interface layer level curved surface and and plane, described zirconia ceramic slurry is not melting mutually, namely whiteruss mutually in, molecule because of two-phase interface layer receives the asymmetric reactive force of two-phase and makes interfacial layer spherically, shape glomerate zirconium dioxide ball-milling medium green compact.
It should be noted that, due to acrylamide and N, N
,-methylene-bisacrylamide in atmosphere time, easily affected by the oxygen contained in air, as the normal formation of gel can be affected, in order to ensure preparing quality better zirconium dioxide ball-milling medium green compact, such as, under vacuum, spray art is adopted described zirconia ceramic slurry and described catalyzer to be sprayed with the form of drop respectively, and after making both droplets mixings, spray into in described oil phase forming agent simultaneously, can guarantee to prepare quality better zirconium dioxide ball-milling medium green compact.
Further, sprayed by above-mentioned raw materials by spray art, what can make to mix between raw material is more even, and more can disperse and more uniformly enter in described whiteruss, is beneficial to follow-uply to obtain submillimeter level zirconium dioxide ball-milling medium described in other.
S160: by filtering, wash and after drying, obtaining prefabricated zirconium dioxide ball-milling medium green compact,
By filtering, washing and drying operation, prefabricated zirconium dioxide ball-milling medium green compact can be separated with oil phase forming agent, to obtain purer prefabricated zirconium dioxide ball-milling medium green compact.
In one embodiment, adopt tetracol phenixin to carry out described washing operation, like this, whiteruss can be removed completely, obtain purer prefabricated zirconium dioxide ball-milling medium green compact.Preferably, the temperature that described drying operation adopts is 80 DEG C ~ 100 DEG C, and the time that described drying operation continues is 18 hours ~ 24 hours, like this, is beneficial to and is removed by tetracol phenixin described in described prefabricated zirconium dioxide ball-milling medium green compact.
And for example, described tetracol phenixin is adopted to carry out repeatedly described washing operation; Described filter operation is vacuum filtration, like this, can remove the described tetracol phenixin in described prefabricated zirconium dioxide ball-milling medium green compact further.
S170: after described prefabricated zirconium dioxide ball-milling medium green sintering, obtain the described zirconium dioxide ball-milling medium of submillimeter level.
After described prefabricated zirconium dioxide ball-milling medium green sintering, namely carry out binder removal process, e.g., discharge organic substance in described prefabricated zirconium dioxide ball-milling medium green compact, to obtain described zirconium dioxide ball-milling medium.
It should be noted that, by above-mentioned preparation method, the described zirconium dioxide ball-milling medium of submillimeter level can be obtained, and can guarantee that the median particle diameter of described zirconium dioxide ball-milling medium is 0.1mm ~ 0.3mm, to meet the demand of ultra-fine ball milling.
In one embodiment, described sintering temperature is 260 DEG C ~ 540 DEG C, like this, and can by the organic compound combustion volatilization in described prefabricated zirconium dioxide ball-milling medium green compact, that is, the random netted organic compound combustion volatilization will be dispersed with equably in described prefabricated zirconium dioxide ball-milling medium green compact.Like this, the density of the described zirconium dioxide ball-milling medium obtained can reach 5.5 ~ 6.5g/cm
3, relative volume density can reach 98% ~ 99%.
The preparation method of the above-mentioned zirconium dioxide ball-milling medium based on gel injection system utilizes the reactive force between two-phase interface can obtain the described zirconium dioxide ball-milling medium of submillimeter level, relative to traditional preparation method, there is the simpler and lower-cost advantage of preparation technology.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1., based on a preparation method for the zirconium dioxide ball-milling medium of gel injection system, it is characterized in that, comprise the steps:
Yttrium is provided to stablize tetragonal phase zirconium oxide powder, deionized water, linking agent, monomer, dispersion agent, initiator, facilitate agent and oil phase forming agent;
Described monomer, described linking agent, described dispersion agent and described deionized water and stirring are mixed, obtains prewired mixed solution;
Described prewired mixed solution and described yttrium are stablized after tetragonal phase zirconium oxide powder mixes, be added to after carrying out ball milling operation in ball grinder, obtain prewired slurry;
After described prewired slurry is mixed with described initiator, be added to after carrying out ball milling operation in ball grinder, obtain zirconia ceramic slurry;
Adopt spray art described zirconia ceramic slurry and described catalyzer to be sprayed with the form of drop respectively, and after making both droplets mixings, spray into in described oil phase forming agent simultaneously;
By filtering, wash and after drying, obtaining prefabricated zirconium dioxide ball-milling medium green compact, wherein, tetracol phenixin is adopted to carry out described washing operation;
After described prefabricated zirconium dioxide ball-milling medium green sintering, obtain the described zirconium dioxide ball-milling medium of submillimeter level.
2. the preparation method of the zirconium dioxide ball-milling medium based on gel injection system according to claim 1, it is characterized in that, described dispersion agent comprises at least one in ammonium citrate and ammonium polyacrylate.
3. the preparation method of the zirconium dioxide ball-milling medium based on gel injection system according to claim 2, is characterized in that, described dispersion agent is ammonium citrate.
4. the preparation method of the zirconium dioxide ball-milling medium based on gel injection system according to claim 1, is characterized in that, adopts described tetracol phenixin to carry out repeatedly described washing operation.
5. the preparation method of the zirconium dioxide ball-milling medium based on gel injection system according to claim 1, is characterized in that, described filter operation is vacuum filtration.
6. the preparation method of the zirconium dioxide ball-milling medium based on gel injection system according to claim 1, is characterized in that, the median particle diameter of the described zirconium dioxide ball-milling medium of submillimeter level is 0.1mm ~ 0.3mm.
7. the preparation method of the zirconium dioxide ball-milling medium based on gel injection system according to claim 1, is characterized in that, the time that described drying operation continues is 18 hours ~ 24 hours.
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| CN109129820A (en) * | 2018-09-29 | 2019-01-04 | 南昌大学 | A kind of pneumatic printing prepares ceramic microsphere device and method |
| CN111302791A (en) * | 2020-02-24 | 2020-06-19 | 东莞市永笃纳米科技有限公司 | Zirconia micro-bead and preparation method thereof |
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| CN111646506A (en) * | 2020-07-21 | 2020-09-11 | 宁德三祥纳米新材料有限公司 | Method for preparing nano zirconium oxide by internal gel method |
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