CN113045319B - Sintering aid modified nano ceramic powder and preparation method thereof - Google Patents
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Abstract
The invention discloses sintering aid modified nano ceramic powder and a preparation method thereof, and relates to the technical field of ceramic materials. The preparation method of the sintering aid modified nano ceramic powder comprises the following steps: (1) Dissolving a sintering aid salt in an organic solvent, adding a dispersing agent, and stirring until the dispersing agent is completely dissolved to obtain a solution A; the sintering aid salt is a salt containing crystal water; (2) Adding the ceramic powder into the solution A, and carrying out ultrasonic and homogeneous mixing to obtain a suspension B; (3) Dropwise adding an organic alkali solution into the stirred suspension B to obtain a modified suspension C; (4) And carrying out ball milling, washing, drying and calcining on the modified suspension C to obtain the sintering aid modified nano ceramic powder. The invention is based on the dissolving and ionizing principles, takes organic solution as solvent, and the modified ceramic powder sintering aid is uniformly coated and almost has no secondary agglomeration.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to sintering aid modified nano ceramic powder and a preparation method thereof.
Background
The preparation process of the ceramic comprises the steps of preparing, forming and sintering a blank. Sintering is a key step for preparing ceramic parts, and a series of physical and chemical changes, volume reduction, density increase, strength and hardness improvement, crystal grain phase change and the like can occur in the ceramic during sintering, so that the ceramic blank body can achieve the required physical property and mechanical property. Sintering can be divided into solid-phase sintering and liquid-phase sintering, generally the same raw material is adopted, and the temperature required by the solid-phase sintering is higher, so that the liquid-phase sintering is a more common sintering method, low-temperature liquid-phase sintering of ceramics is generally realized by adding a sintering aid, and the sintering aid is also called a sintering aid and has the functions of 1) forming a solid solution with a sintering object to promote lattice distortion activation; 2) Prevent the volume effect generated by the lattice transformation; 3) Inhibiting the growth of crystal grains; 4) A liquid phase is generated, promoting particle rearrangement and mass transfer processes.
The common addition method of ceramic sintering aid mainly adopts main phase ceramicThe common ball milling and mixing mode of the porcelain powder requires that the particle size of the auxiliary agent is close to that of the main phase ceramic, the ball milling time is long, but the mixing effect is still not ideal; secondly, the main phase ceramic powder is added into the sintering aid suspension or gel, but the sintering aid can generate self agglomeration under the action of capillary force, and the sintering aid effect is difficult to realize; thirdly, sintering additive salt (TiCl) 4 Or ZrCl 4 ) Dissolving in ethanol, mixing with main phase ceramic powder under stirring, removing solvent, and forming nanometer coating (TiO) on the surface of the main phase ceramic powder 2 Or ZrO 2 ) However, toxic gases and chlorine residues are usually generated during the solvent removal process, resulting in the formation of pores due to gas emission from the ceramic during sintering.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides sintering aid modified nano ceramic powder and a preparation method thereof based on a dissolution and ionization mechanism.
In order to realize the purpose, the technical scheme adopted by the invention is as follows: a preparation method of sintering aid modified nano ceramic powder comprises the following steps:
(1) Dissolving a sintering aid salt in an organic solvent, adding a dispersing agent, and stirring until the dispersing agent is completely dissolved to obtain a solution A; the sintering aid salt is a salt containing crystal water;
(2) Adding ceramic powder into the solution A, and carrying out ultrasonic and homogeneous mixing to obtain a suspension B;
(3) Dropwise adding an organic alkali solution into the stirred suspension B until the pH value is equal to the isoelectric point of the sintering aid hydroxide, and continuously stirring to obtain a modified suspension C;
(4) And performing ball milling, washing, drying and calcining on the modified suspension C to obtain the sintering aid modified nano ceramic powder.
The invention is based on the basic theories of dissolution and ionization, namely sintering aid salt is dissolved in an organic solvent and ionized in water, crystal water is adsorbed on the surface of the main-phase ceramic powder, the sintering aid salt is ionized in the water, hydroxide or complex hydroxide precipitate is generated on the surface of the main-phase ceramic powder under the action of alkali, and the sintering aid modified nano ceramic powder is obtained through drying and calcining; in the product, the sintering aid is uniformly distributed on the ceramic powder.
Preferably, in the step (1), the sintering aid salt comprises at least one of yttrium nitrate hexahydrate, yttrium chloride hydrate, aluminum nitrate nonahydrate, aluminum chloride hexahydrate, calcium nitrate tetrahydrate, calcium chloride dihydrate, magnesium nitrate hexahydrate, magnesium chloride hexahydrate, and lanthanum nitrate hexahydrate; the organic solvent comprises at least one of methanol, ethanol, acetone, n-hexane, petroleum ether and benzene.
Preferably, in the sintering aid modified nano ceramic powder, the content of the sintering aid is 1 to 20wt.% of the sintering aid modified nano ceramic powder.
Preferably, in the step (2), the ceramic powder body contains at least one of alumina, zirconia, silicon carbide, silicon nitride and aluminum nitride.
Preferably, in the step (3), the volume ratio of the organic base to the organic solvent in the organic base solution is 1.
Further preferably, in the step (3), the volume ratio of the organic base to the organic solvent in the organic base solution is 1. When the concentration of the organic base in the organic base solution is too high, the precipitated particles are too large, and the mechanical properties of the ceramic are greatly influenced.
Preferably, the organic base comprises at least one of methylamine, ethylenediamine, dimethylamine, triethylamine, aniline.
Preferably, in the step (4), the ball milling of the modified suspension C is carried out for 2-12 h, and the organic solvent washing is carried out for 2-6 times.
Meanwhile, the invention also discloses the sintering aid modified nano ceramic powder prepared by the method.
Compared with the prior art, the invention has the beneficial effects that: the sintering aid salt is dissolved in an organic solvent and ionized in water, crystal water is adsorbed on the surface of the main-phase ceramic powder, the sintering aid is ionized in water, hydroxide or complex hydroxide precipitate is generated on the surface of the main-phase ceramic powder under the action of alkali, and the mixed ceramic powder coated and modified by the sintering aid is obtained through washing, drying and calcining. Compared with the traditional ball-milling mixing method of the sintering aid and the main phase ceramic powder, the method has better mixing effect and lower time cost; compared with the method of adding the main phase ceramic powder into the sintering aid suspension or gel, the distribution of the sintering aid is more uniform; compared with a method of dissolving the sintering aid in an organic solvent, stirring and mixing the organic solvent with the main-phase ceramic powder, and finally removing the solvent, the method is more environment-friendly, and avoids pores formed inside the ceramic blank body due to residue of acid radicals in the sintering process by washing and removing anions; in addition, the organic solution is used as a solvent, so that hard agglomeration of the ceramic powder due to a large amount of hydroxyl groups in the calcining process is avoided.
Drawings
FIG. 1 is a TEM image and an EDS image of elements of the sintering aid modified nano ceramic powder of example 2;
FIG. 2 is a TEM image of the sintering aid-modified nano ceramic powder and an EDS image of elements in comparative example 2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
In an embodiment of the present invention, a method for preparing a sintering aid-modified nano ceramic powder includes the following steps:
(1) Dissolving lanthanum nitrate hexahydrate in ethanol, and dissolving a dispersant PEG2000 in the ethanol to obtain a solution A;
(2) Gradually adding silicon nitride ceramic powder into the solution A, carrying out ultrasonic treatment for 3 minutes, carrying out homogeneous mixing at 2000 rpm for 1 minute, and repeating for 3 times to obtain a suspension B;
(3) Dropwise adding an organic alkali solution with the volume ratio of methylamine to ethanol being 1 into the stirring suspension B until the pH value is 9-9.5, and continuously stirring for 2 hours to obtain a modified suspension C;
(4) Ball-milling the modified suspension C for 2 hours, washing for 3 times, drying, and calcining at 500 ℃ for 1 hour to obtain uniformly coated silicon nitride ceramic powder;
wherein, the dosage of lanthanum nitrate hexahydrate and silicon nitride is added according to the mass ratio of lanthanum oxide to silicon nitride of 3.
Tests show that the La element is uniformly distributed on the surface of the powder.
Example 2
In an embodiment of the present invention, a method for preparing a sintering aid-modified nano ceramic powder includes the following steps:
(1) Dissolving yttrium nitrate hexahydrate in acetone, and dissolving a dispersing agent in the acetone to obtain a solution A;
(2) Gradually adding silicon carbide ceramic powder into the solution A, carrying out ultrasonic treatment for 5 minutes, carrying out homogeneous mixing for 2 minutes at 1000 revolutions per minute, and repeating for 2 times to obtain a suspension B;
(3) Dropwise adding an organic alkali solution with the volume ratio of ethylenediamine to acetone being 1;
(4) Ball-milling the modified suspension C for 4 hours, washing for 2 times, drying, and calcining at 600 ℃ for 1 hour to obtain uniformly-coated silicon carbide ceramic powder;
wherein the dosage of the yttrium nitrate hexahydrate and the silicon carbide is as follows: silicon carbide mass ratio = 5.
Fig. 1 is a TEM image and an EDS image of elements of the sintering aid modified nano ceramic powder in this embodiment, and it can be seen from fig. 1 that the Y element is uniformly distributed on the surface of the silicon carbide particle, indicating that the sintering aid forms an effective coating on the surface of the ceramic powder.
Example 3
In an embodiment of the present invention, a method for preparing a sintering aid modified nano ceramic powder includes the following steps:
(1) Dissolving yttrium nitrate hexahydrate and magnesium nitrate hexahydrate in petroleum ether, and dissolving a dispersing agent in the petroleum ether to obtain a solution A;
(2) Gradually adding silicon carbide ceramic powder into the solution A, carrying out ultrasonic treatment for 3 minutes, carrying out 1500 rpm homogeneous mixing for 3 minutes, and repeating the steps for 3 times to obtain a suspension B;
(3) Adding an organic alkali solution with the volume ratio of methylamine to petroleum ether being 1;
(4) Ball-milling the modified suspension C for 6 hours, washing for 6 times, drying, and calcining at 700 ℃ for 1 hour to obtain uniformly-coated silicon carbide ceramic powder;
wherein the dosage of the yttrium nitrate hexahydrate, the magnesium nitrate hexahydrate and the silicon carbide is as follows: magnesium oxide: silicon carbide mass ratio = 4.
Tests show that the Y element and the Mg element are uniformly distributed on the surface of the powder.
Comparative example 1
A preparation method of sintering aid modified nano ceramic powder comprises the following steps:
(1) Dissolving yttrium nitrate hexahydrate in a mixed solvent of acetone and water (volume ratio of 1;
(2) Gradually adding silicon carbide ceramic powder into the solution A, carrying out ultrasonic treatment for 3 minutes, carrying out homogeneous mixing for 1 minute at 2500 rpm, and carrying out reciprocating treatment for 2 times to obtain a suspension B;
(3) Aqueous ammonia (75 wt.% NH) 3 ·H 2 O) dropwise adding the mixture into the suspension B under stirring until the pH value is 9-9.5, and continuously stirring for 2 hours to obtain a modified suspension C;
(4) Ball-milling the modified suspension C for 4 hours, washing for 2 times, drying, and calcining at 600 ℃ for 1 hour to obtain sintering aid modified nano ceramic powder;
wherein, the dosage of the yttrium nitrate hexahydrate and the silicon carbide ceramic powder is added according to the mass ratio of yttrium oxide to silicon carbide of 3.
Tests show that the Y element can not be dispersed on the surface of the powder, and the agglomeration phenomenon occurs.
Comparative example 2
A preparation method of sintering aid modified nano ceramic powder comprises the following steps:
(1) Dissolving yttrium nitrate hexahydrate in deionized water, and dissolving a dispersing agent in the deionized water to obtain a solution A;
(2) Gradually adding silicon carbide ceramic powder into the solution A, carrying out ultrasonic treatment for 5 minutes, carrying out homogeneous mixing at 1000 rpm for 2 minutes, reciprocating for 2 times, and lasting for 1 hour to obtain a suspension B;
(3) Dropwise adding an organic alkali solution with the volume ratio of ethylenediamine to acetone being 1;
(4) Ball-milling the modified suspension C for 2 hours, washing for 2 times, drying, and calcining at 600 ℃ for 1 hour to obtain sintering aid modified nano ceramic powder;
wherein, the dosage of the yttrium nitrate hexahydrate and the silicon carbide ceramic powder is added according to the mass ratio of yttrium oxide to silicon carbide of 3.
Tests prove that the sintering aid modified nano ceramic powder in the comparative example is agglomerated, and Y does not form effective coating on the surfaces of silicon carbide particles. FIG. 2 is a TEM image and an EDS image of elements of the sintering aid-modified nano-ceramic powder of this comparative example, and it can be seen from FIG. 2 that the distribution of Y elements on the surface of the silicon carbide particles is small, indicating that Y is present 2 O 3 Not coated on the silicon carbide surface.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (5)
1. A preparation method of sintering aid modified nano ceramic powder is characterized by comprising the following steps:
(1) Dissolving a sintering aid salt in an organic solvent, adding a dispersing agent, and stirring until the dispersing agent is completely dissolved to obtain a solution A; the sintering aid salt is a salt containing crystal water;
(2) Adding the ceramic powder into the solution A, and carrying out ultrasonic and homogeneous mixing to obtain a suspension B;
(3) Dropwise adding an organic alkali solution into the stirred suspension B until the pH value is equal to the isoelectric point of the sintering aid hydroxide, and continuously stirring to obtain a modified suspension C;
(4) Carrying out ball milling, washing, drying and calcining on the modified suspension C to obtain the sintering aid modified nano ceramic powder;
in the step (3), in the organic alkali solution, the volume ratio of the organic alkali to the organic solvent is 1;
in the step (4), ball-milling the modified suspension C for 2-12 h, and washing with an organic solvent for 2-6 times;
in the step (1), the sintering aid salt comprises at least one of yttrium nitrate hexahydrate, yttrium chloride hydrate, aluminum nitrate nonahydrate, aluminum chloride hexahydrate, calcium nitrate tetrahydrate, calcium chloride dihydrate, magnesium nitrate hexahydrate, magnesium chloride hexahydrate and lanthanum nitrate hexahydrate; the organic solvent comprises at least one of methanol, ethanol, acetone, n-hexane, petroleum ether and benzene.
2. The preparation method of claim 1, wherein the content of the sintering aid in the sintering aid modified nano ceramic powder is 1wt.% to 20wt.% of the sintering aid modified nano ceramic powder.
3. The method according to claim 1, wherein in the step (2), the ceramic powder body contains at least one of alumina, zirconia, silicon carbide, silicon nitride, and aluminum nitride.
4. The method of any one of claims 1 to 3, wherein the organic base comprises at least one of methylamine, ethylenediamine, dimethylamine, triethylamine, aniline.
5. A sintering aid modified nano ceramic powder prepared by the method of any one of claims 1 to 4.
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