CN111286217B - Cobalt blue sepiolite nano composite pigment, preparation method and application thereof - Google Patents
Cobalt blue sepiolite nano composite pigment, preparation method and application thereof Download PDFInfo
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- CN111286217B CN111286217B CN201811500132.5A CN201811500132A CN111286217B CN 111286217 B CN111286217 B CN 111286217B CN 201811500132 A CN201811500132 A CN 201811500132A CN 111286217 B CN111286217 B CN 111286217B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B17/00—Insulators or insulating bodies characterised by their form
- H01B17/56—Insulating bodies
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a preparation method of a cobalt blue sepiolite nano composite pigment, which comprises the following steps: mixing water-soluble cobalt salt and aluminum salt, and dissolving in water to obtain a mixed solution; adjusting the pH value of the mixed solution to 12-14 and stirring; adding organic nano sepiolite into the mixed solution, stirring to obtain a uniform suspension solution, then carrying out hydrothermal reaction on the suspension solution with stirring, and carrying out post-treatment on a product obtained by the reaction to obtain the powdery cobalt blue sepiolite nano composite pigment. The preparation method of the cobalt blue sepiolite nano composite pigment selects water-soluble cobalt salt and aluminum salt as raw materials, takes organic nano sepiolite fiber as a heterogeneous nucleation center, and synthesizes the cobalt blue sepiolite nano composite pigment by a kinetic control coating method under the condition of hydrothermal stirring.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to a cobalt blue sepiolite composite pigment, a preparation method thereof and application thereof in thick film dielectric paste.
Background
The thick film dielectric paste is a functional coating material which appears along with the development of thick film circuit technology, and is generally formed by mixing glass phase powder and an organic carrier according to a certain proportion, forming a coating on the surface of a substrate by screen printing when in use, and drying and sintering under a certain heat treatment process. In recent years, with the wide application of thick film circuit technology in the fields of communication equipment and household appliances, thick film coatings with good thermal stability, bright color and smooth surface are more and more favored by the market.
Cobalt blue is a metal oxide mixed phase pigment with spinel crystal structure, and the chemical composition of the cobalt blue is mainly CoO and A12O3Or called cobalt aluminate (CoAl)2O4) In the "pigment index," the name is pigment 28. CobaltThe excellent performance of the blue pigment is mainly shown in excellent weather resistance, acid and alkali resistance, high thermal stability and chemical stability. In addition, the cobalt blue pigment is also obviously superior to other blue pigments in the aspects of transparency, saturation, chroma, refractive index and the like, and belongs to a nontoxic environment-friendly pigment. Thus, cobalt blue is considered to be the most suitable pigment for thick film coatings.
When cobalt blue pigment is compounded with thick film slurry for use, the dispersion stability of pigment particles in an organic vehicle is very important for obtaining a high-performance thick film coating. The preparation of the cobalt blue sold in the market at present generally needs high temperature treatment at the temperature of more than 1000 ℃, so the particle size of the cobalt blue pigment is generally larger, and the cobalt blue pigment is easy to agglomerate and settle when being compounded with an organic carrier due to the inorganic material property of the cobalt blue pigment, so the insulation and thermal shock resistance of a thick film coating are influenced.
Disclosure of Invention
The invention mainly aims to provide a cobalt blue sepiolite nano composite pigment and a preparation method thereof, so as to overcome the defects in the prior art.
The invention also aims to provide application of the cobalt blue sepiolite nanocomposite pigment.
In order to achieve the purpose, the invention adopts the following technical scheme:
the embodiment of the invention provides a preparation method of a cobalt blue sepiolite nano composite pigment, which comprises the following steps:
(1) mixing water-soluble cobalt salt and aluminum salt, and dissolving in water to obtain a mixed solution;
(2) adjusting the pH value of the mixed solution to 12-14 and stirring;
(3) and (3) adding organic nano sepiolite into the mixed solution obtained in the step (2), stirring to obtain a uniform suspension solution, carrying out hydrothermal reaction on the suspension solution with stirring, and carrying out post-treatment on a product obtained by the reaction to obtain the powdery cobalt blue sepiolite nano composite pigment.
The embodiment of the invention also provides the cobalt blue sepiolite nano composite pigment prepared by the method.
The embodiment of the invention also provides application of the cobalt blue sepiolite nano composite pigment in thick film dielectric paste or a thick film composite coating.
The embodiment of the invention also provides a preparation method of the thick film dielectric paste, which comprises the following steps: ball milling is carried out on the cobalt blue sepiolite nano composite pigment and borosilicate glass powder, mixed powder after ball milling is placed in an organic carrier consisting of terpineol and ethyl cellulose, and thick film medium slurry is prepared by grinding, wherein the cobalt blue sepiolite nano composite pigment is the cobalt blue sepiolite nano composite pigment.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the cobalt blue sepiolite nano composite pigment provided by the embodiment of the invention has the advantages of simple process, low synthesis temperature, no need of subsequent high-temperature heat treatment and low preparation energy consumption.
(2) The cobalt blue sepiolite nano composite pigment obtained by the invention is nano particles, has the characteristics of small size, good dispersibility and fibrous micro morphology, has good suspension stability in an organic carrier, and is beneficial to screen printing forming.
(3) The cobalt blue sepiolite nano composite pigment prepared by the invention is used for preparing a coating in thick film dielectric paste, and has uniform and bright color, and the insulation strength and the thermal shock resistance are obviously improved.
(4) One of the raw materials used in the invention is sepiolite which is a natural mineral resource and has the advantages of wide material source, green and safe property, low application cost and the like.
Detailed Description
Aiming at the defects of the prior art, the inventor of the invention provides the technical scheme of the invention through long-term research and massive practice. The technical solution, its implementation and principles, etc. will be further explained as follows. It is to be understood, however, that within the scope of the present invention, each of the above-described features of the present invention and each of the features described in detail below (examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.
As one aspect of the technical scheme of the invention, the preparation method of the cobalt blue sepiolite nano composite pigment comprises the following steps:
(1) mixing water-soluble cobalt salt and aluminum salt, and dissolving in water to obtain a mixed solution;
(2) adjusting the pH value of the mixed solution to 12-14 and stirring;
(3) and (3) adding organic nano sepiolite into the mixed solution obtained in the step (2), stirring to obtain a uniform suspension solution, carrying out hydrothermal reaction on the suspension solution with stirring, and carrying out post-treatment on a product obtained by the reaction to obtain the powdery cobalt blue sepiolite nano composite pigment.
In some embodiments, step (1) comprises: stirring the mixed solution at a speed of 200-500 rpm for 30-50 min.
In some embodiments, step (2) specifically comprises: dripping 2-4 mol/L NaOH solution into the mixed solution to adjust the pH value of the mixed solution to 12-14, and stirring the mixed solution at the speed of 200-500 r/min for 8-15 hours.
In some embodiments, step (3) specifically comprises: adding organic nano sepiolite into the mixed solution obtained in the step (2), stirring for 2-5 hours at the speed of 200-500 r/min to obtain a uniform suspension solution, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with a stirrer, and cooling to room temperature after the hydrothermal reaction is finished.
In some embodiments, the hydrothermal reaction is carried out at a temperature of 230 to 250 ℃ for 15 to 20 hours.
In some embodiments, the post-treatment comprises: and centrifugally washing the obtained product by using a mixed solution of deionized water and alcohol in a mass ratio of 1-2: 1, and drying the obtained product for 10-20 hours to obtain the powdery cobalt blue sepiolite nano composite pigment.
In some embodiments, the water-soluble cobalt salt comprises cobalt chloride and/or cobalt nitrate and the water-soluble aluminum salt comprises aluminum chloride and/or aluminum nitrate.
In some embodiments, the organic nano sepiolite is selected from nano sepiolite fibers which are 0.5-1 um long and 25-40 nm in diameter and are modified by phenylsilane.
In some embodiments, the mass ratio of the organic nano sepiolite to the cobalt element is 5-10: 1.
In some embodiments, the mixed solution is Co2+With Al3+The molar ratio of (A) to (B) is 1: 2.
In some specific embodiments, a method for preparing a cobalt blue sepiolite nanocomposite pigment comprises:
mixing water-soluble cobalt salt and aluminum salt, dissolving in deionized water, stirring for 30-50 min at the speed of 200-500 r/min, dripping prepared 2-4 mol/L NaOH solution into the mixed solution to adjust the pH value to 12-14, stirring for 8-15 h at the speed of 200-500 r/min, adding organic nano-sepiolite with a certain mass, stirring for 2-5 h at the speed of 200-500 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for a plurality of hours at a high temperature, cooling to room temperature, repeatedly centrifuging and washing a product by using the deionized water and alcohol mixed solution with the mass ratio of 1-2: 1, and then placing in a vacuum drying oven for drying for 10-20 h to obtain the cobalt blue sepiolite composite powder.
The embodiment of the invention also provides a cobalt blue sepiolite nano composite pigment prepared by the method.
The embodiment of the invention also provides application of the cobalt blue sepiolite nano composite pigment in thick film dielectric paste or a thick film composite coating.
The embodiment of the invention also provides a preparation method of the thick film dielectric paste, which comprises the following steps: ball milling is carried out on the cobalt blue sepiolite nano composite pigment and borosilicate glass powder, mixed powder after ball milling is placed in an organic carrier consisting of terpineol and ethyl cellulose, and thick film medium slurry is prepared by grinding, wherein the cobalt blue sepiolite nano composite pigment is the cobalt blue sepiolite nano composite pigment.
In some embodiments, the mass ratio of the borosilicate glass powder to the cobalt blue sepiolite nanocomposite pigment is 5-10: 1.
In some embodiments, the mass ratio of the terpineol to the cobalt blue sepiolite nanocomposite pigment in the organic vehicle is 2-3: 1.
The mass ratio of the ethyl cellulose to the cobalt blue sepiolite nano composite pigment in the organic carrier is 0.3-0.5: 1.
In some specific embodiments, a method of making a thick film dielectric paste comprises:
and (2) placing the cobalt blue sepiolite nano composite pigment and the borosilicate glass powder in a ball milling tank for ball milling for 2 hours, placing the ball-milled mixed powder in an organic carrier consisting of terpineol and ethyl cellulose, and grinding by a three-roll grinder to prepare thick film medium slurry.
According to the preparation method of the cobalt blue sepiolite nano composite pigment provided by the embodiment of the invention, water-soluble cobalt salt and aluminum salt are selected as raw materials, organic nano sepiolite fibers are used as heterogeneous nucleation centers, and the cobalt blue sepiolite nano composite pigment is synthesized by a kinetic control coating method under the condition of hydrothermal stirring; and the cobalt blue sepiolite thick film composite coating with excellent performance is obtained by effective compounding with thick film slurry.
The technical solutions of the present invention will be described in further detail with reference to several preferred embodiments, and it should be apparent 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 obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The conditions used in the following examples may be further adjusted as necessary, and the conditions used in the conventional experiments are not generally indicated.
Example 1:
mixing and dissolving 0.1mol of cobalt chloride and 0.2mol of aluminum chloride in 1000ml of deionized water, stirring for 50min at the speed of 200 r/min, dripping 2mol/L of prepared NaOH solution into the mixed solution to adjust the pH value to 12, stirring for 15h at the speed of 200 r/min, then adding organic nano-sepiolite with the mass of 10 times of that of cobalt element, stirring for 5h at the speed of 200 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for 20h at 230 ℃, cooling to room temperature, repeatedly centrifuging and washing a product by using a deionized water and alcohol mixed solution with the mass ratio of 1: 1, and then placing the product in a vacuum drying oven to dry for 10h to obtain the cobalt blue sepiolite composite pigment.
10g of the prepared cobalt blue sepiolite nano composite pigment and borosilicate glass powder with the mass 5 times that of the cobalt blue sepiolite nano composite pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol with the mass 2 times that of the cobalt blue sepiolite nano composite pigment and ethyl cellulose with the mass 0.5 time that of the cobalt blue sepiolite nano composite pigment and is ground by a three-roll grinder to prepare thick film medium slurry.
Example 2:
mixing and dissolving 0.1mol of cobalt chloride and 0.2mol of aluminum chloride in 1000ml of deionized water, stirring for 30min at the speed of 500 r/min, dripping prepared 4mol/L of NaOH solution into the mixed solution to adjust the pH value to 14, stirring for 8h at the speed of 500 r/min, then adding organic nano-sepiolite with the mass 5 times that of cobalt element, stirring for 5h at the speed of 500 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for 15h at 250 ℃, cooling to room temperature, repeatedly centrifuging and washing a product by using a deionized water and alcohol mixed solution with the mass ratio of 2:1, and then placing the product in a vacuum drying oven to dry for 20h to obtain the cobalt blue sepiolite composite pigment.
10g of the prepared cobalt blue sepiolite nano composite pigment and borosilicate glass powder with the mass 10 times that of the cobalt blue sepiolite nano composite pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol with the mass 3 times that of the cobalt blue sepiolite nano composite pigment and ethyl cellulose with the mass 0.3 time that of the cobalt blue sepiolite nano composite pigment and is ground by a three-roll grinder to prepare thick film medium slurry.
Example 3:
mixing and dissolving 0.1mol of cobalt chloride and 0.2mol of aluminum chloride in 1000ml of deionized water, stirring for 40min at the speed of 350 r/min, dripping the prepared 3mol/L NaOH solution into the mixed solution to adjust the pH value to 13, stirring for 11h at the speed of 300 r/min, then adding organic nano-sepiolite with the mass of 8 times of that of cobalt element, stirring for 2h at the speed of 350 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for 18h at 240 ℃, cooling to room temperature, repeatedly centrifuging and washing a product by using the mixed solution of the deionized water and the alcohol with the mass ratio of 1.5: 1, and then placing the product in a vacuum drying oven to dry for 15h to obtain the cobalt blue sepiolite composite pigment.
10g of the prepared cobalt blue sepiolite nano composite pigment and borosilicate glass powder with the mass 8 times that of the cobalt blue sepiolite nano composite pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol with the mass 2.5 times that of the cobalt blue sepiolite nano composite pigment and ethyl cellulose with the mass 0.4 time that of the cobalt blue sepiolite nano composite pigment and is ground by a three-roll grinder to prepare thick film medium slurry.
Example 4:
mixing and dissolving 0.1mol of cobalt nitrate and 0.2mol of aluminum nitrate in 1000ml of deionized water, stirring for 40min at the speed of 300 r/min, dripping 2.5mol/L of prepared Na0H solution into the mixed solution to adjust the pH value to 12, stirring for 8h at the speed of 300 r/min, then adding organic nano-sepiolite with the mass being 7 times that of cobalt element, stirring for 3h at the speed of 300 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for 18h at 250 ℃, cooling to room temperature, repeatedly centrifuging and washing a product by using the mixed solution of the deionized water and the alcohol with the mass ratio of 1: 1, and then placing the product in a vacuum drying oven to dry for 13h to obtain the cobalt blue sepiolite composite powder.
10g of the prepared cobalt blue sepiolite nano composite pigment and borosilicate glass powder 7 times the mass of the cobalt blue sepiolite nano composite pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol 2.4 times the mass of the cobalt blue sepiolite nano composite pigment and ethyl cellulose 0.5 times the mass of the cobalt blue sepiolite nano composite pigment and is ground into thick film medium slurry by a three-roll grinder.
Example 5:
mixing and dissolving 0.1mol of cobalt chloride and 0.2mol of aluminum nitrate in 1000ml of deionized water, stirring for 50min at the speed of 400 r/min, dripping 3mol/L of prepared Na0H solution into the mixed solution to adjust the pH value to 13, stirring for 11h at the speed of 350 r/min, then adding organic nano sepiolite with the mass of 9 times of cobalt element, stirring for 5h at the speed of 350 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for 18h at 250 ℃, cooling to room temperature, repeatedly centrifuging and washing a product by using the mixed solution of the deionized water and the alcohol with the mass ratio of 2:1, and then placing the product in a vacuum drying oven to dry for 15h to obtain the cobalt blue sepiolite composite powder.
10g of the prepared cobalt blue sepiolite nano composite pigment and borosilicate glass powder 6 times the mass of the cobalt blue sepiolite nano composite pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol 2.5 times the mass of the cobalt blue sepiolite nano composite pigment and ethyl cellulose 0.4 times the mass of the cobalt blue sepiolite nano composite pigment and is ground into thick film medium slurry by a three-roll grinder.
Example 6:
mixing and dissolving 0.1mol of cobalt nitrate and 0.2mol of aluminum chloride in 1000ml of deionized water, stirring for 40min at the speed of 300 r/min, dripping 2mol/L of prepared Na0H solution into the mixed solution to adjust the pH value to 12, stirring for 12h at the speed of 350 r/min, then adding organic nano-sepiolite with the mass of 6 times of cobalt element, stirring for 5h at the speed of 350 r/min, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with stirring, reacting for 19h at 260 ℃, cooling to room temperature, repeatedly centrifuging and washing a product by using the mixed solution of deionized water and alcohol with the mass ratio of 1.5: 1, and then placing the product in a vacuum drying oven to dry for 20h to obtain the cobalt blue sepiolite composite powder.
10g of the prepared cobalt blue sepiolite nano composite pigment and borosilicate glass powder with the mass 5 times that of the cobalt blue sepiolite nano composite pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol with the mass 2 times that of the cobalt blue sepiolite nano composite pigment and ethyl cellulose with the mass 0.5 time that of the cobalt blue sepiolite nano composite pigment and is ground by a three-roll grinder to prepare thick film medium slurry.
Comparative example 1:
10g of commercially available micron-sized cobalt blue pigment prepared by a traditional solid phase method and borosilicate glass powder with the mass 5 times that of the micron-sized cobalt blue pigment are placed in a ball milling tank for ball milling for 2 hours, and the ball-milled mixed powder is placed in an organic carrier consisting of terpineol with the mass 2 times that of the micron-sized cobalt blue pigment and ethyl cellulose with the mass 0.5 time that of the micron-sized cobalt blue pigment and is ground into thick film medium slurry by a three-roll grinder.
And (3) performance characterization:
the thick film insulating pastes obtained in examples 1 to 6 and comparative example 1 were printed on the surface of a stainless steel substrate by a screen printer, followed by heat treatment at 850 ℃ in a mesh belt flash furnace to form a 100 μm thick film coating, and then the insulating properties and thermal shock resistance of the coating were characterized as shown in table 1, where table 1 is test data of the insulating properties and thermal shock resistance of the thick film coatings obtained in examples 1 to 6 and comparative example 1.
Table 1.
Sample (I) | Insulation resistance M omega | Breakdown voltage kV | Thermal shock gradient (. DELTA.T) deg.C |
Example 1 | 65.8 | 2.4 | 550 |
Example 2 | 64.6 | 2.2 | 550 |
Example 3 | 64.2 | 2.3 | 550 |
Example 4 | 65.4 | 2.4 | 550 |
Example 5 | 64.6 | 2.3 | 550 |
Example 6 | 65.7 | 2.2 | 550 |
Comparative example 1 | 47.6 | 1.8 | 350 |
As can be seen from the data in Table 1, the insulating property and the thermal shock resistance of the thick film coating obtained by using the cobalt blue sepiolite nano composite pigment prepared by the invention are greatly improved.
In addition, the inventor also carries out corresponding tests by using other process conditions and the like listed in the foregoing to replace the corresponding process conditions in the examples 1 to 6, and the contents to be verified are similar to the products of the examples 1 to 6. Therefore, the contents of the verification of each example are not described herein one by one, and only examples 1 to 6 are used as representatives to describe the excellent points of the present invention.
It should be noted that, in the present document, in a general case, an element defined by the phrase "includes.
It should be understood that the above-mentioned examples are only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and to implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. The preparation method of the thick film dielectric paste is characterized by comprising the following steps:
(1) mixing water soluble cobalt salt and aluminum salt, dissolving in water to obtain mixed solution, wherein Co2+With Al3+In a molar ratio of 1: 2;
(2) adjusting the pH value of the mixed solution to 12-14 and stirring;
(3) adding organic nano sepiolite into the mixed solution obtained in the step (2), wherein the mass ratio of the organic nano sepiolite to cobalt elements is 5-10: 1, the organic nano sepiolite is selected from nano sepiolite fibers which are 0.5-1 um long and 25-40 nm in diameter and are modified by phenyl silane, stirring to obtain a uniform suspension solution, then carrying out hydrothermal reaction on the suspension solution with stirring, the temperature of the hydrothermal reaction is 230-250 ℃, the time is 15-20 hours, and carrying out post-treatment on a product obtained by the reaction to obtain a powdery cobalt blue sepiolite nano composite pigment;
(4) ball milling is carried out on the cobalt blue sepiolite nano composite pigment and borosilicate glass powder, wherein the mass ratio of the borosilicate glass powder to the cobalt blue sepiolite nano composite pigment is 5-10: 1, the ball milled mixed powder is placed into an organic carrier consisting of terpineol and ethyl cellulose, the mass ratio of the terpineol to the cobalt blue sepiolite nano composite pigment in the organic carrier is 2-3: 1, the mass ratio of the ethyl cellulose to the cobalt blue sepiolite nano composite pigment in the organic carrier is 0.3-0.5: 1, and thick film medium slurry is prepared through grinding.
2. The method according to claim 1, wherein the step (1) comprises: stirring the mixed solution at a speed of 200-500 rpm for 30-50 min.
3. The method according to claim 1, wherein the step (2) specifically comprises: dripping 2-4 mol/L NaOH solution into the mixed solution to adjust the pH value of the mixed solution to 12-14, and stirring the mixed solution at the speed of 200-500 r/min for 8-15 hours.
4. The method according to claim 1, wherein the step (3) specifically comprises: adding organic nano sepiolite into the mixed solution obtained in the step (2), stirring for 2-5 hours at the speed of 200-500 r/min to obtain a uniform suspension solution, transferring the uniformly stirred suspension solution into a hydrothermal reaction kettle with a stirrer, and cooling to room temperature after the hydrothermal reaction is finished.
5. The method of manufacturing according to claim 1, wherein the post-treatment comprises: and centrifugally washing the obtained product by using a mixed solution of deionized water and alcohol in a mass ratio of 1-2: 1, and drying the obtained product for 10-20 hours to obtain the powdery cobalt blue sepiolite nano composite pigment.
6. The method of claim 1, wherein: the water-soluble cobalt salt comprises cobalt chloride and/or cobalt nitrate, and the water-soluble aluminum salt comprises aluminum chloride and/or aluminum nitrate.
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Anjie Zhang,et al..Cobalt blue hybrid pigment doped with magnesium derived from sepiolite.《Applied Clay Science》.2018, * |
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