CN112708301A - Preparation method of nano 8YSZ aqueous phase suspension with stable dispersion - Google Patents
Preparation method of nano 8YSZ aqueous phase suspension with stable dispersion Download PDFInfo
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- 229910002080 8 mol% Y2O3 fully stabilized ZrO2 Inorganic materials 0.000 title claims abstract description 89
- 239000000725 suspension Substances 0.000 title claims abstract description 79
- 239000006185 dispersion Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000008346 aqueous phase Substances 0.000 title abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000007790 solid phase Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000007900 aqueous suspension Substances 0.000 claims description 52
- 229920001223 polyethylene glycol Polymers 0.000 claims description 29
- 239000003153 chemical reaction reagent Substances 0.000 claims description 27
- 239000002202 Polyethylene glycol Substances 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- -1 Polypropylene Polymers 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000003607 modifier Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 31
- 230000000694 effects Effects 0.000 abstract description 27
- 239000002105 nanoparticle Substances 0.000 abstract description 14
- 239000002086 nanomaterial Substances 0.000 abstract description 11
- 230000002776 aggregation Effects 0.000 abstract description 5
- 230000007246 mechanism Effects 0.000 abstract description 5
- 230000006641 stabilisation Effects 0.000 abstract description 4
- 238000011105 stabilization Methods 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 3
- 230000009977 dual effect Effects 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 7
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000006070 nanosuspension Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 3
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- 239000012720 thermal barrier coating Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
本发明涉及纳米材料分散技术领域，尤其是涉及的是一种分散稳定的纳米8YSZ水相悬浮液的制备方法，包括以下步骤：称取纳米8YSZ粉末，加入去离子水，搅拌均匀，得到固相质量分数为10％～30％的悬浮初液；将分散剂加入到该悬浮初液中，进行分散处理，得到悬浮液。本发明通过添加了分散剂，使得悬浮液中形成静电稳定与空间位阻的双重机制，来实现纳米粒子的分散。其中，静电稳定机制是在颗粒表面形成一种双电层的结构，粒子表面同种电荷相互排斥，实现分散效果；空间位阻机制是通过分散剂吸附于纳米粒子表面，使得相邻颗粒上的聚合物因体积效应而相斥，提高了纳米颗粒聚集必须克服的能量势垒，从而实现粒子在悬浮液中的分散。
The invention relates to the technical field of nanomaterial dispersion, in particular to a method for preparing a nano-8YSZ aqueous phase suspension with stable dispersion, comprising the following steps: weighing nano-8YSZ powder, adding deionized water, stirring evenly, and obtaining a solid phase The initial suspension liquid whose mass fraction is 10% to 30%; the dispersant is added to the initial suspension liquid, and the dispersion treatment is carried out to obtain the suspension liquid. The invention realizes the dispersion of nanoparticles by adding a dispersant to form a dual mechanism of electrostatic stabilization and steric hindrance in the suspension. Among them, the electrostatic stabilization mechanism is to form an electric double layer structure on the surface of the particles, and the same charges on the particle surface repel each other to achieve the dispersion effect; The polymers are repelled by volume effects, raising the energy barrier that must be overcome for nanoparticle aggregation to achieve particle dispersion in suspension.
Description
Technical Field
The invention relates to the technical field of nano material dispersion, in particular to a preparation method of a nano 8YSZ aqueous phase suspension with stable dispersion.
Background
Y2O3(8YSZ) is a high-temperature-resistant oxide, has the characteristics of high melting point, high hardness, low thermal conductivity and the like, and is widely applied to thermal spraying to prepare high-performance Thermal Barrier Coatings (TBCs). The nano particles have the characteristics of large specific surface area, small size effect, interface and surface effect, quantum size effect and the like, and have excellent performances which cannot be compared with a plurality of conventional particles in the aspects of catalysis, optics, magnetism, mechanics and the like, so that the nano particles have wide application prospects. The composite coating containing the nano structure is prepared by combining the nano material with a surface coating technology and adopting a suspension plasma spraying process, has potential excellent performance of the nano material, and can improve the using effect of the coating.
The nano powder suspension with low viscosity and good dispersion stability is a precondition for suspension plasma spraying. Due to the lack of adjacent coordinating atoms on the surface of the nanoparticles, the large specific surface area and the high surface energy, the individual nanoparticles tend to be in an unstable state and spontaneously agglomerate due to mutual attraction. The generation of the phenomenon reduces the specific surface and the surface activity, thereby losing the specific functions of the nano powder. Therefore, the dispersion of the nanoparticles in the aqueous suspension is a critical factor.
At present, the method for dispersing the nanoparticles in the suspension is mainly a mechanical method. The mechanical method is ultrasonic oscillation or ball milling, the two-phase dispersion system obtained by the method is a thermodynamically unstable system, particles meet again after a certain time to generate agglomeration, the dispersion effect is not durable, and the excellent performance of the nano material is reduced.
Disclosure of Invention
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The invention aims to overcome the defects and provide a preparation method of nano 8YSZ aqueous phase suspension with stable dispersion, the preparation method is simple, the viscosity of particles in the prepared nano 8YSZ aqueous phase suspension is low, the potential is high, no agglomeration is generated among the particles, the dispersion system is stable, the dispersion effect is good, the excellent performance of the nano 8YSZ is greatly improved, and the nano 8YSZ is more widely applied to coatings.
In order to achieve the purpose, the technical solution of the invention is as follows: a preparation method of a dispersion-stable nano 8YSZ aqueous phase suspension comprises the following steps:
s1, preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a suspension primary solution with a solid phase mass fraction of 10-30%;
s2, dispersion of the suspension: adding a dispersing agent into the primary suspension, and performing dispersion treatment to obtain a suspension;
s3, adjusting the pH value of the suspension: and adding a pH regulator into the suspension for pH value regulation to obtain the suspension with the pH value of 7-9.
Preferably, the pH regulator is hydrochloric acid and ammonia water.
Preferably, the dispersing agent is a polyethylene glycol reagent (PEG for short) with the mass fraction of 0-4%.
Preferably, the polyethylene glycol reagent is one or two of polyethylene glycol reagent with molecular weight of 600 and polyethylene glycol reagent with molecular weight of 2000.
Preferably, the dispersant is a polyethylene glycol reagent with the mass fraction of 2.4%.
Preferably, the dispersant is a polyethylene glycol reagent with the mass fraction of 3.2%.
Preferably, the dispersant is 0-4% of polypropylene reagent (PAA) by mass fraction.
Preferably, the dispersant is a polypropylene agent with a mass fraction of 2.4%.
Preferably, the particle size of the nano 8YSZ powder is 20nm to 60 nm.
By adopting the technical scheme, the invention has the beneficial effects that:
1. according to the invention, the dispersing agent is added, so that a double mechanism of electrostatic stabilization and steric hindrance is formed in the suspension, and the dispersion of the nano particles is realized. Wherein, the electrostatic stabilization mechanism is that a double electric layer structure is formed on the particle surface, and the same charges on the particle surface repel each other to realize the dispersion effect; the steric hindrance mechanism is that the dispersing agent is adsorbed on the surface of the nano particles, so that polymers on adjacent particles repel each other due to the volume effect, and the energy barrier which must be overcome by the aggregation of the nano particles is improved, thereby realizing the dispersion of the particles in the suspension.
2. After the dispersing agent is added, the pH value of the suspension is adjusted, so that the potential of the nano particles in the suspension is highest, the viscosity among particles in the suspension is reduced to the lowest, and the dispersing effect among the particles is realized.
3. The preparation method is simple, the viscosity of the particles in the prepared nano 8YSZ water phase suspension is low, the potential is high, no agglomeration is generated between the particles, the dispersion system is stable, the dispersion effect is good, the excellent performance of the nano 8YSZ is greatly improved, and the application of the nano 8YSZ is wider.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
Clearly, such objects and other objects of the present invention will become more apparent from the detailed description of the preferred embodiments hereinafter set forth in the various drawings and drawings.
These and other objects, features and advantages of the present invention will become more apparent from the following detailed description of one or more preferred embodiments of the invention, as illustrated in the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings, like parts are designated with like reference numerals, and the drawings are schematic and not necessarily drawn to scale.
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, it is obvious that the drawings in the following description are only one or several embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to such drawings without creative efforts.
FIG. 1 is a first flow chart of a method for preparing a dispersion-stabilized aqueous suspension of nano 8YSZ according to the present invention;
FIG. 2 is a second flow chart of the method of preparing a dispersion-stabilized aqueous suspension of nano 8YSZ according to the present invention;
FIG. 3 is a graph showing the effect of PEG600 content in a dispersion-stabilized aqueous suspension of nano 8YSZ on the viscosity of the aqueous suspension of nano 8YSZ in accordance with the present invention;
FIG. 4 is a graph of the effect of PEG2000 content in a dispersion-stabilized aqueous suspension of nano 8YSZ on the viscosity of the aqueous suspension of nano 8YSZ in accordance with the present invention;
FIG. 5 is a graph of the effect of PEG content in a dispersion-stabilized aqueous suspension of nano 8YSZ on the viscosity of the aqueous suspension of nano 8YSZ in accordance with the present invention;
FIG. 6 is a graph showing the effect of pH on zeta potential for PAA dispersion in a dispersion stabilized aqueous suspension of nano 8YSZ in accordance with the present invention;
FIG. 7 is a graph showing the effect of pH on suspension viscosity under PAA dispersion in a dispersion-stabilized aqueous suspension of nano 8YSZ in accordance with the present invention;
FIG. 8 is a third flow chart of a method for preparing a dispersion-stabilized aqueous suspension of nano 8 YSZ;
FIG. 9 is a graph showing the effect of pH on zeta potential in a dispersion stabilized aqueous suspension of nano 8YSZ without dispersant;
fig. 10 is a graph showing the particle size distribution of a dispersion-stabilized aqueous suspension of nano 8YSZ at PH 8, without a dispersing agent.
Detailed Description
The following detailed description of the embodiments of the present invention will be provided with reference to the drawings and examples, so that how to apply the technical means to solve the technical problems and achieve the technical effects can be fully understood and implemented. It should be noted that, as long as there is no conflict, the embodiments and the features of the embodiments of the present invention may be combined with each other, and the technical solutions formed are within the scope of the present invention.
In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the embodiments of the invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced without some of these specific details or with other methods described herein.
Example 1
Referring to fig. 1, fig. 1 is a first flow chart of a method for preparing a stable dispersed nano 8YSZ aqueous suspension according to the present invention.
The implementation provides a preparation method of a nano 8YSZ aqueous phase suspension with stable dispersion, which comprises the following steps:
s1, preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a primary suspension with a solid phase mass fraction of 20%;
s2, dispersion of the suspension: and adding a dispersing agent into the primary suspension for dispersing treatment to obtain a suspension.
The dispersing agent is a polyethylene glycol reagent (PEG for short) with the mass fraction of 0-4%, the polyethylene glycol reagent is a polyethylene glycol reagent (PEG 600 for short) with the molecular weight of 600, the grade of the polyethylene glycol reagent is chemical purity, and the polyethylene glycol reagent is provided by the chemical reagent company of the national drug group.
The nanometer 8YSZ powder has particle diameter of 40nm and specific surface area of 25m2Per g, from Nanjing seaTai nano materials ltd.
The grade of the deionized water was three.
Referring to fig. 3, fig. 3 is a graph showing the effect of PEG600 content in a dispersion-stabilized nano 8YSZ aqueous suspension on the viscosity of a nano 8YSZ aqueous suspension according to the present invention.
The viscosity of the nano 8YSZ aqueous suspension was measured by using a DV-III — ULTRA rheometer manufactured by Brookfield (boehlefei) in usa, and the dispersion stability of the nano 8YSZ aqueous suspension was determined by the viscosity under the conditions of a rotor model of 61, a rotation speed of 150r/min, and a room temperature, and the measurement results are shown in fig. 3.
As can be seen from fig. 3, when the dispersant is PEG600 with a mass fraction of 3.2%, the viscosity of the nano 8YSZ aqueous suspension prepared in this example is 4.08mpa.s, and is the lowest, and the nano 8YSZ aqueous suspension is stable in dispersion.
Example 2
Referring to fig. 1, fig. 1 is a first flow chart of a method for preparing a stable dispersed nano 8YSZ aqueous suspension according to the present invention.
The implementation provides a preparation method of a nano 8YSZ aqueous phase suspension with stable dispersion, which comprises the following steps:
s1, preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a primary suspension with a solid phase mass fraction of 20%;
s2, dispersion of the suspension: and adding a dispersing agent into the primary suspension for dispersing treatment to obtain a suspension.
The dispersing agent is a polyethylene glycol reagent (PEG for short) with the mass fraction of 0-4%, the polyethylene glycol reagent is a polyethylene glycol reagent (PEG 2000 for short) with the molecular weight of 2000, the grade of the polyethylene glycol reagent is chemical purity, and the polyethylene glycol reagent is provided by the chemical reagent company of the national drug group.
The nanometer 8YSZ powder has particle diameter of 40nm and specific surface area of 25m2(ii)/g, provided by Nanjing Haitai Nano materials, Inc.
The grade of the deionized water was three.
Referring to fig. 4, fig. 4 is a graph showing the effect of PEG2000 content in a dispersion-stabilized nano 8YSZ aqueous suspension on the viscosity of a nano 8YSZ aqueous suspension according to the present invention.
The viscosity of the nano 8YSZ aqueous suspension was measured by using a DV-III — ULTRA rheometer manufactured by Brookfield (boehlefei) in usa, and the dispersion stability of the nano 8YSZ aqueous suspension was determined by the viscosity under the conditions of a rotor model of 61, a rotation speed of 150r/min, and a room temperature, and the measurement results are shown in fig. 4.
As can be seen from fig. 4, when the dispersant is PEG2000 with a mass fraction of 2.4%, the viscosity of the nano 8YSZ aqueous suspension prepared in this example is 3.84mpa.s, and is the lowest, and the nano 8YSZ aqueous suspension is stable in dispersion.
Example 3
Referring to fig. 1, fig. 1 is a first flow chart of a method for preparing a stable dispersed nano 8YSZ aqueous suspension according to the present invention.
The implementation provides a preparation method of a nano 8YSZ aqueous phase suspension with stable dispersion, which comprises the following steps:
s1, preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a primary suspension with a solid phase mass fraction of 20%;
s2, dispersion of the suspension: and adding a dispersing agent into the primary suspension for dispersing treatment to obtain a suspension.
The dispersing agent is a polypropylene reagent (PAA for short) with the mass fraction of 0-4%, the grade of the PAA is chemical purity, and the PAA is provided by Tai and water treatment Co.
The nanometer 8YSZ powder has particle diameter of 40nm and specific surface area of 25m2(ii)/g, provided by Nanjing Haitai Nano materials, Inc.
The grade of the deionized water was three.
Referring to fig. 5, fig. 5 is a graph showing the effect of PEG content in a dispersion-stabilized nano 8YSZ aqueous suspension on the viscosity of a nano 8YSZ aqueous suspension according to the present invention.
The viscosity of the nano 8YSZ aqueous suspension was measured by using a DV-III — ULTRA rheometer manufactured by Brookfield (boehlefei) in usa, and the dispersion stability of the nano 8YSZ aqueous suspension was determined by the viscosity under the conditions of a rotor model of 61, a rotation speed of 150r/min, and a room temperature, and the measurement results are shown in fig. 5.
As can be seen from fig. 5, when the dispersant is PAA with a mass fraction of 2.4%, the viscosity of the nano 8YSZ aqueous suspension prepared in this example is 3.36mpa.s, and is the lowest, and the nano 8YSZ aqueous suspension is stable in dispersion.
Example 4
Referring to fig. 2, fig. 2 is a flow chart of a preparation method of a dispersion-stabilized nano 8YSZ aqueous suspension according to the present invention.
The implementation provides a preparation method of a nano 8YSZ aqueous phase suspension with stable dispersion, which comprises the following steps:
s1, preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a primary suspension with a solid phase mass fraction of 20%;
s2, dispersion of the suspension: adding a dispersing agent into the primary suspension, and performing dispersion treatment to obtain a suspension;
s3, adjusting the pH value of the suspension: a pH adjusting agent is added to the suspension to adjust the pH.
The pH regulator is hydrochloric acid and ammonia water, has analytical purity in the grade, and is provided by chemical reagents of national drug group, Inc.
The dispersant was a polypropylene reagent (PAA for short) having a mass fraction of 2.4%, and the grade thereof was chemically pure and was provided by tai, shandong province and water treatment limited.
The nanometer 8YSZ powder has particle diameter of 40nm and specific surface area of 25m2(ii)/g, provided by Nanjing Haitai Nano materials, Inc.
The grade of the deionized water was three.
Referring to FIG. 6, FIG. 6 is a graph showing the effect of pH on zeta potential under PAA dispersion in a dispersion-stabilized aqueous nano-8 YSZ suspension according to the present invention.
The Zeta potential of the nano 8YSZ particles in the aqueous suspension of nano 8YSZ was measured by a model Js94H microelectrophoresis apparatus, and the results of the measurement are shown in table 1 and fig. 6.
TABLE 1 influence of the pH on the zeta potential of the nanosuspension particles under PAA Dispersion
As can be seen from table 1 and fig. 6, when the dispersant is PAA with a mass fraction of 2.4% and the PH is 8, the Zeta potential of the nano 8YSZ particles in the nano 8YSZ aqueous suspension prepared in this example in water is-44.5, and is the highest, and the nano 8YSZ aqueous suspension is stable in dispersion.
Referring to fig. 7, fig. 7 is a graph showing the effect of PH on the viscosity of a dispersion stabilized aqueous suspension of PAA in a nano 8YSZ of the present invention.
The viscosity of the nano 8YSZ aqueous suspension was measured by using a Brookfield (boehlefei) DV-III — ULTRA rheometer, and the dispersion stability of the nano 8YSZ aqueous suspension was determined by the viscosity under the conditions of a rotor type of 61, a rotation speed of 150r/min, and a room temperature, and the measurement results are shown in table 2 and fig. 7.
TABLE 2 influence of pH on the viscosity of nanosuspensions in PAA Dispersion
As can be seen from table 2 and fig. 7, when the dispersant is PAA with a mass fraction of 2.4% and the PH is 8, the viscosity of the nano 8YSZ aqueous suspension prepared in this example is 2.56, and is the lowest, and the nano 8YSZ aqueous suspension is stable in dispersion.
Example 5
Referring to fig. 8, fig. 8 is a flow chart of a third process for preparing a dispersion-stabilized nano 8YSZ aqueous suspension.
The implementation provides a preparation method of a nano 8YSZ aqueous phase suspension with stable dispersion, which comprises the following steps:
s1, preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a primary suspension with a solid phase mass fraction of 20%;
s2, adjusting the pH value of the suspension: a pH adjusting agent is added to the suspension to adjust the pH.
The pH regulator is hydrochloric acid and ammonia water, has analytical purity in the grade, and is provided by chemical reagents of national drug group, Inc.
The nanometer 8YSZ powder has particle diameter of 40nm and specific surface area of 25m2(ii)/g, provided by Nanjing Haitai Nano materials, Inc.
The grade of the deionized water was three.
Referring to fig. 9, fig. 9 is a graph showing the effect of PH on zeta potential in a dispersion stabilized aqueous nano 8YSZ suspension without dispersant.
The Zeta potential of the nano 8YSZ particles in the aqueous suspension of nano 8YSZ was measured using a model Js94H microelectrophoresis apparatus, and the results of the measurement are shown in table 3 and fig. 9.
TABLE 3 Effect of pH on zeta potential of nanosuspension particles without addition of dispersant
Referring to fig. 10, fig. 10 is a graph showing the particle size distribution of a dispersion-stabilized aqueous suspension of nano 8YSZ at PH 8 without a dispersing agent.
The viscosity of the nano 8YSZ aqueous suspension was measured by using a Brookfield (boehlefei) DV-III — ULTRA rheometer, and the dispersion stability of the nano 8YSZ aqueous suspension was judged from the viscosity under the conditions of a rotor type of 61, a rotation speed of 150r/min, and a room temperature, and the measurement results are shown in table 4 and fig. 10.
TABLE 4 particle size distribution of suspension at pH 8 without dispersant addition
From tables 3 and 4, it can be seen that the zeta potential is the largest when the isoelectric point pH of the nano 8YSZ is equal to 6 and the pH is 8. The pH value is only adjusted without adding a dispersing agent, so that the suspension cannot be stably dispersed, and the suspension nanoparticles are agglomerated and have larger particle size.
In summary, from examples 1-3, the overall dispersion effect is PAA > PEG2000> PEG 600. Different dispersants are used in a certain amount, and too much dispersant can reduce the dispersion stability of the suspension.
From example 4, it can be seen that the dispersion effect is better than that of examples 1-3, when 2.4 wt.% of dispersing agent PAA is added, the pH value of isoelectric point of nano 8YSZ is equal to 4, the zeta potential at pH 8 is maximum-44.5, and the viscosity of suspension is minimum 2.56 mpa.s.
From example 5, it can be seen that the zeta potential is maximal at pH 8 at isoelectric point pH of 8 nm YSZ equal to 6. The pH value is only adjusted without adding a dispersing agent, so that the suspension cannot be stably dispersed, and the suspension nanoparticles are agglomerated and have larger particle size.
It is to be understood that the disclosed embodiments of the invention are not limited to the particular process steps or materials disclosed herein, but rather, are extended to equivalents thereof as would be understood by those of ordinary skill in the relevant art. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting.
Reference in the specification to "an embodiment" means that a particular feature, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. Thus, the appearances of the phrase or "an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment.
It should be noted that in the foregoing description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and thus the scope of the present invention is not limited by the specific embodiments disclosed above.
Claims (10)
1. A preparation method of a nano 8YSZ aqueous suspension with stable dispersion is characterized by comprising the following steps:
preparing a suspension initial solution: weighing nano 8YSZ powder, adding deionized water, and uniformly stirring to obtain a suspension primary solution with a solid phase mass fraction of 10-30%;
dispersion of the suspension: and adding a dispersing agent into the primary suspension for dispersing treatment to obtain a suspension.
2. The method of preparing the dispersion-stabilized nano 8YSZ aqueous suspension of claim 1, further comprising the steps of:
adjustment of the pH of the suspension: and adding a pH regulator into the suspension for pH value regulation to obtain the suspension with the pH value of 7-9.
3. The method of claim 2, wherein the PH modifier is hydrochloric acid or ammonia.
4. The method for preparing the dispersion-stabilized nano 8YSZ aqueous suspension according to claim 1, wherein the dispersant is 0-4% by mass of polyethylene glycol (PEG).
5. The method of claim 4, wherein the polyethylene glycol reagent is one or a combination of polyethylene glycol reagent with molecular weight of 600 and polyethylene glycol reagent with molecular weight of 2000.
6. The method of claim 4, wherein the dispersing agent is 2.4 wt% polyethylene glycol.
7. The method of claim 4, wherein the dispersant is 3.2 wt% polyethylene glycol.
8. The method of claim 1, wherein the dispersant is 0-4% by weight of Polypropylene (PAA) reagent.
9. The method of claim 6, wherein the dispersing agent is 2.4% polypropylene agent.
10. The method of claim 1, wherein the size of the nano 8YSZ powder is 20nm to 60 nm.
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