CN113683403B - Alumina slurry for nitrogen-oxygen sensor and preparation method thereof - Google Patents
Alumina slurry for nitrogen-oxygen sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses alumina slurry for a nitrogen-oxygen sensor and a preparation method thereof. The obtained slurry has good fineness, cannot be scribed by particles in an F.O.G scraper fineness meter, can adapt to 325-mesh screen printing, effectively reduces the powder removal phenomenon, is simple to operate and is easy for mass production.
Description
Technical Field
The invention relates to an alumina slurry for a nitrogen-oxygen sensor and a preparation method thereof, belonging to the field of alumina slurry.
Background
With the continuous development of information technology, the electronic technology is continuously updated, and the research and development of corresponding electronic materials are rapidly developed. Alumina slurry has attracted attention as an important material for a nitrogen oxygen sensor because of its excellent insulating properties and thermal conductivity.
At present, alumina slurry applied in more quantity in the market is still monopolized by foreign manufacturers, and the alumina slurry produced in China generally has the defects of poor dispersibility, poor printing, poor drying state and the like, and is not enough to meet the performance requirements of the alumina slurry.
The invention provides an alumina slurry and a preparation method thereof, and is particularly suitable for the field of nitrogen-oxygen sensors, aiming at the technical problems that in the existing alumina slurry, the alumina powder is poor in dispersion (the fineness is more than 13 in the slurry), screen printing cannot be carried out, the printing thickness is insufficient and the like.
Disclosure of Invention
The invention aims to provide alumina slurry for a nitrogen-oxygen sensor and a preparation method thereof, and solves the technical problems that the existing alumina slurry is poor in split dispersibility, cannot be subjected to screen printing and the like.
A preparation method of alumina slurry for a nitrogen-oxygen sensor is characterized in that wet ball milling technology is adopted to prepare alumina powder, and an organic carrier is combined to obtain silk-screen alumina slurry.
The preparation method specifically comprises the following steps:
(1) Mixing the alumina powder, the dispersant and the solvent, and adding the zirconium balls to obtain the mixed material.
The dispersing agent is one or more of polyethylene wax, polyvinyl alcohol, organic silicon, urea, TDO, NANOCHE ED120 and BYK-410 (all of which are commercially available), and the polyethylene wax is preferred.
The D50 of the alumina powder is 0.1-0.7 μm.
The solvent is selected from one or more of volatile alcohols (such as ethanol and propanol), ketones and ethers, preferably alcohols.
In the mixed material, the adding amount of the alumina powder is 60-70 parts by weight, the adding amount of the dispersant is 1-5 parts by weight, and the adding amount of the solvent is 100-150 parts by weight.
The diameter of the zirconium balls is 0.5-1.5mm.
The mass of the zirconium balls is 60-85wt% of the mixed material.
The polyethylene wax has better compatibility with the alumina powder, has a certain lubricating function, and has fewer precipitates.
Preferably, the amount of dispersant added is M (dispersant): m (alumina) = (1-7): 84, more preferably (2-4): 84.
too much dispersant will cause the subsequent alumina to agglomerate easily, and conversely too little dispersant will cause the alumina powder not to maintain a stable suspension system, so the dispersant dosage needs to be strictly controlled.
(2) And ball-milling the obtained mixed material, and then filtering, drying and sieving to obtain the alumina powder.
The ball milling revolution is 200-500R/min, and the ball milling time is 1-5 hours.
The filter was into a stainless steel vessel.
And the drying is to preserve heat for 3-5h at the temperature of 60-90 ℃ in an oven, and dry the filtered sample.
The sieve is 50-200 meshes.
(3) Preparing an organic carrier: mixing solvent and resin, and water bath at 60-70 deg.C for 1-2 hr to obtain organic carrier with concentration of 15-25 wt%.
The solvent is selected from alcohol ester dodeca, terpineol or a eutectic solvent, and is preferably a eutectic solvent.
The eutectic solvent is choline chloride or consists of betaine and urea according to the molar ratio of 1:2. The choline chloride or the betaine are used as hydrogen bond acceptors, the urea is used as a hydrogen bond donor, and the organic resin is pretreated by virtue of the action of the hydrogen bond, so that the uniformity of initial slurry is facilitated, the strength and the performance of the carrier are improved, and the silk-screen printing effect is improved.
The resin is polyvinyl butyral (PVB) and/or cellulose resin, such as ethyl cellulose and cellulose acetate butyrate;
preferably polyvinyl butyral, in combination with a cellulosic resin, wherein PVB: the mass ratio of the cellulose resin is (2-4): 1, the powder removal phenomenon of the slurry can be further reduced.
(4) And mixing the prepared organic carrier, the alumina powder and the organic solvent, and stirring to obtain initial slurry.
Wherein, based on 100 percent of the initial slurry, the content of the organic carrier accounts for 10 to 20 weight percent, the content of the alumina powder accounts for 60 to 70 weight percent, and the balance is organic solvent.
The organic solvent is alcohol ester dodeca, terpineol or ethylene glycol butyl ether acetate.
The stirring refers to manual stirring or stirring by adopting a homogenizer.
(5) Rolling: and (4) rolling the initial slurry obtained in the step (4) for 5-8 times by using a rolling mill, so that the slurry is dispersed more uniformly.
The rolling mill is a zirconia three-high rolling mill.
The invention also provides alumina slurry obtained by the preparation method.
Further, the present invention also provides a nitrogen oxygen sensor using the alumina slurry obtained by the above preparation method, which has good fineness and no grain line visible in an f.o.g. blade fineness gauge.
The invention has the beneficial effects that:
1. according to the invention, through controlling the types and the adding amount of polyethylene wax serving as a dispersing agent and a grinding solvent, the particle size of the alumina powder and other parameters, the dispersibility of the alumina powder becomes good in the ball milling process; the fineness was good in the slurry, and no particle streaks were visible in the f.o.g. blade fineness gauge.
2. The invention optimizes the ball milling process and improves the ball milling efficiency by controlling the diameter and the mass ratio of the zirconium balls.
3. According to the invention, the alumina slurry suitable for 325-mesh screen printing can be obtained by using a suitable organic resin, and the powder removal phenomenon is effectively reduced.
4. The method for treating the alumina powder has simple operation and is easy for mass production.
5. The alumina slurry prepared by the invention has good dispersity, does not agglomerate after being dried, has good screen printing effect and uniform thickness, and can meet the use requirement.
6. The invention improves the dispersion performance of the slurry by solvation of the organic carrier, and is beneficial to improving the silk-screen effect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the application and together with the description serve to explain the principles of the application.
Fig. 1 is a drawing of an f.o.g. screed of a slurry prepared in example 1 of the present invention.
Fig. 2 is a drawing of an f.o.g. screed of a slurry prepared according to example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 4g of polyethylene wax, 110g of ethanol (99%) and 500g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
(2) Separating the ball-milled materials from the zirconium balls, placing the zirconium balls in a stainless steel box, keeping the temperature in an oven at 80 ℃ for 3 hours, and then passing the dried alumina powder through a 50-mesh stainless steel screen;
(3) Preparing an organic carrier: betaine/urea (molar ratio 1:2) was mixed with PVB resin and water bath at 70 ℃ for 1 hour to prepare an organic vehicle with a concentration of 18.8 wt%.
(4) Fully mixing 12.8g of powder obtained by sieving, 2.98g of PVB carrier and 3.82g of terpineol to obtain initial slurry;
(5) And rolling the initial slurry for 8 times by using a zirconia three-high mill to obtain the required alumina slurry.
Example 2
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 2g of polyethylene wax, 110g of ethanol (99%) and 600g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
(2) Separating the ball-milled material from the zirconium balls, placing the ball-milled material in a stainless steel box, keeping the temperature in an oven at 80 ℃ for 3h, drying, and then passing the dried alumina powder through a 50-mesh stainless steel screen;
(3) Preparing an organic carrier: betaine/urea (molar ratio 1:2) was mixed with PVB resin and water bath at 70 ℃ for 1 hour to prepare an organic vehicle with a concentration of 18.8 wt%.
(4) Fully mixing 12.8g of powder obtained by sieving, 2.92g of PVB carrier and 3.88g of terpineol to obtain initial slurry;
(5) And rolling the initial slurry for 8 times by using a zirconia three-high mill to obtain the required alumina slurry.
Example 3
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 6.6g of polyethylene wax, 110g of ethanol (99%) and 600g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
the other steps were the same as in example 1 to obtain the desired alumina slurry.
Example 4
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 1.3g of polyethylene wax, 110g of ethanol (99%) and 600g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
the other steps were the same as in example 1 to obtain the desired alumina slurry.
Example 5
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
the other steps are the same as example 1, except that: (4) And fully mixing 12.8g of powder obtained by sieving, 2g of PVB carrier and 4g of terpineol to obtain initial slurry.
Finally obtaining the required alumina slurry.
Example 6
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
the other steps are the same as example 1, except that: (4) And fully mixing 12.8g of powder obtained by sieving, 4g of PVB carrier and 4g of terpineol to obtain initial slurry.
Finally obtaining the required alumina slurry.
Example 7
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 4g of polyethylene wax, 130g of alcohol (99%), and 550g of 1mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 500R/min;
(2) Separating the ball-milled material from the zirconium balls, placing the ball-milled material in a stainless steel box, keeping the temperature in an oven at 100 ℃ for 3 hours, and then passing the dried alumina powder through a 60-mesh stainless steel screen;
(3) Preparing an organic carrier: betaine/urea (molar ratio 1:2) was mixed with PVB resin and water bath at 70 ℃ for 1 hour to prepare an organic vehicle with a concentration of 18.8 wt%.
(4) Fully mixing 12.8g of powder obtained by sieving, 2.98g of PVB carrier and 3.82g of terpineol to obtain initial slurry;
(5) And (4) rolling the initial slurry for 6 times by using a zirconia three-high mill to obtain the required alumina slurry.
Example 8
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
the other steps are the same as example 1, except that: (3) preparing an organic carrier: mixing betaine/urea (molar ratio 1:2) with 20 parts by weight of PVB and 10 parts by weight of ethyl cellulose fiber, so that the mass ratio of the PVB to the ethyl cellulose fiber is 2:1, in a water bath at 70 ℃ for 1 hour, an organic vehicle was prepared at a concentration of 18.8% by weight.
Finally obtaining the required alumina slurry.
Example 9
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
the other steps are the same as in example 1, except that: (3) preparing an organic carrier: mixing betaine/urea (molar ratio 1:2) with 40 parts by weight of PVB and 10 parts by weight of ethyl cellulose fiber, so that the mass ratio of the PVB to the ethyl cellulose fiber is 4:1, in a water bath at 70 ℃ for 1 hour, an organic vehicle was prepared at a concentration of 18.8% by weight.
Finally obtaining the required alumina slurry.
Example 10
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 4g of polyethylene wax, 110g of ethanol (99%) and 500g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
(2) Separating the ball-milled material from the zirconium balls, placing the ball-milled material in a stainless steel box, keeping the temperature in an oven at 80 ℃ for 3h, drying, and then passing the dried alumina powder through a 50-mesh stainless steel screen;
(3) Preparing an organic carrier: choline chloride/urea (molar ratio 1:2) was mixed with PVB resin and water bath at 70 ℃ for 1 hour to prepare an organic vehicle with a concentration of 22 wt%.
(4) Fully mixing 12g of powder obtained by sieving, 2.5g of PVB carrier and 4g of terpineol to obtain initial slurry;
(5) And (4) rolling the initial slurry for 6 times by using a zirconia three-high mill to obtain the required alumina slurry.
Example 11
A preparation method of alumina slurry for a nitrogen-oxygen sensor comprises the following steps:
(1) Placing 84g of alumina, 4g of polyethylene wax, 110g of ethanol (99%) and 500g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
(2) Separating the ball-milled materials from the zirconium balls, placing the zirconium balls in a stainless steel box, keeping the temperature in an oven at 80 ℃ for 3 hours, and then passing the dried alumina powder through a 50-mesh stainless steel screen;
(3) Preparing an organic carrier: the alcohol ester twelve and PVB resin were mixed and water-bathed at 70 ℃ for 1 hour to prepare an organic vehicle having a concentration of 18.8 wt%.
(4) Fully mixing 12.8g of powder obtained by sieving, 2.98g of PVB carrier and 3.82g of terpineol to obtain initial slurry;
(5) And rolling the initial slurry for 8 times by using a zirconia three-high mill to obtain the required alumina slurry.
Comparative example 1
A preparation method of alumina slurry comprises the following steps:
(1) Placing 84g of alumina and 500g of 0.8mm zirconium balls in a polyurethane container, and ball-milling for 2 hours at the speed of 300R/min;
the other steps were the same as in example 1 to obtain an alumina slurry.
Comparative example 2
A preparation method of alumina slurry comprises the following steps:
(1) Placing 84g of alumina, 4g of polyethylene wax, 110g of alcohol (99%) and 500g of 0.8mm zirconium balls in a polyurethane container, and performing ball milling for 2 hours at the speed of 300R/min;
(2) Separating the ball-milled material from the zirconium balls, placing the ball-milled material in a stainless steel box, keeping the temperature in an oven at 80 ℃ for 3h, drying, and then passing the dried alumina powder through a 50-mesh stainless steel screen;
(3) Fully mixing 12.8g of powder obtained by sieving and 3.82g of terpineol to obtain initial slurry;
(4) And rolling the initial slurry for 8 times by using a zirconia three-high mill to obtain the required alumina slurry.
And (3) performance testing:
in the invention, the viscosity test method comprises the following steps: BROOKFIELD DV-II + Pro/CP52 rotors (10 RPM, 25 ℃).
The slurry fineness was measured using an f.o.g. blade fineness gauge (15 μm).
Powder removal rate: the measurement was carried out using a reciprocating abrasion tester (TRIBOGEAR TYPE: 30). For weight W 1 (g) A substrate (2) having a load of 100g/m 2 (contact area 16 mm. Phi.) was pressed against a white cloth, and the cloth was reciprocated 100 times in a width of 5cm, to measure the weight W of the substrate 2 (g) To obtain the powder removal amount (g/m) 2 )。
Powder removal rate (%) = powder removal amount (g/m) 2 ) Weight per unit area (g/m) 2 )×100。
And (3) testing the body resistivity: printing a square block with the area of 10mm-10mm on the outer surface of zirconia by using alumina slurry in a screen printing mode, drying, sintering in a muffle furnace, cooling to normal temperature, testing the sheet resistance by using a four-probe, testing the thickness of the alumina layer by using a step instrument, and obtaining the volume resistivity by calculation.
The results of the performance test of the slurries prepared in the examples and comparative examples are shown in table 1.
Table 1 test of alumina slurry properties
It can be seen from the data of the examples and the comparative examples that the alumina slurry prepared by the invention adopts polyethylene wax as a dispersing agent for ball milling, and combines with an organic carrier, and through carrier modification, the screen printing alumina slurry suitable for 325 meshes can be obtained, the fineness of the slurry is good, and no particle scribing can be seen on an F.O.G scraper fineness meter (as shown in figures 1-2).
The invention controls the adding amount M of the dispersant (dispersant): m (alumina) = (1-7): 84, particularly in (2-4): 84, the effective dispersion of the alumina powder can be kept, and the strength, the particle size and the like of a wet ball milling and subsequent process control system are facilitated;
meanwhile, the modification of the organic carrier, the compounding of the organic carrier and the control of the addition amount can effectively improve the printing stability and uniformity of the slurry, ensure the printing thickness and the printing uniformity and have less powder removal. The eutectic solvent is adopted, so that the eutectic solvent is green, non-toxic and easy to separate, the carrier performance is improved, and the screen printing effect is optimized.
In the description herein, reference to the description of the terms "one embodiment/mode," "some embodiments/modes," "example," "specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/mode or example is included in at least one embodiment/mode or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment/mode or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/aspects or examples and features of the various embodiments/aspects or examples described in this specification can be combined and combined by one skilled in the art without conflicting therewith.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present application, "plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
It should be understood by those skilled in the art that the above embodiments are only for clearly illustrating the present application, and are not intended to limit the scope of the present application. Other variations or modifications will occur to those skilled in the art based on the foregoing disclosure and are still within the scope of the present application.
Claims (7)
1. A preparation method of alumina slurry for a nitrogen-oxygen sensor is characterized in that a wet ball milling process is adopted to mix alumina powder, a dispersant and a solvent, zirconium balls are added for ball milling, then filtering, drying and sieving are carried out, the obtained alumina powder is mixed with an organic carrier, and the alumina slurry is obtained through rolling;
the method specifically comprises the following steps:
(1) Mixing alumina powder, a dispersant and a solvent, and adding zirconium balls to obtain a mixed material;
(2) Ball-milling the obtained mixed material, and then filtering, drying and sieving to obtain alumina powder;
(3) Preparing an organic carrier: mixing a solvent and resin, and preparing an organic carrier with the concentration of 15-25wt% in water bath at 60-70 ℃ for 1-2 hours;
the solvent in the step (3) is selected from alcohol ester dodeca, terpineol or a eutectic solvent, wherein the eutectic solvent is choline chloride or is composed of betaine and urea according to a molar ratio of 1:2;
the resin is polyvinyl butyral (PVB) and cellulose resin; wherein PVB: the mass ratio of the cellulose resin is (2-4): 1, the fiber resin is selected from ethyl cellulose and cellulose acetate butyrate;
(4) Mixing the prepared organic carrier, alumina powder and an organic solvent, and stirring to obtain initial slurry;
(5) Rolling: and (4) rolling the initial slurry obtained in the step (4).
2. The preparation method according to claim 1, wherein the dispersant in the step (1) is one or more of polyethylene wax, polyvinyl alcohol, TDO, NANOCHEMICAL ED120, BYK-410; the D50 of the alumina powder is 0.1-0.7 μm; the solvent is selected from one or more of alcohols, ketones and ethers.
3. The preparation method according to claim 1, wherein the amount of the alumina powder added in the mixed material in the step (1) is 60 to 70 parts by weight, the amount of the dispersant added is 1 to 5 parts by weight, and the amount of the solvent added is 100 to 150 parts by weight.
4. The production method according to claim 3, characterized in that the dispersant is added in an amount of M (dispersant): m (aluminum oxide) = (1-7): 84.
5. The preparation method according to claim 1, wherein the number of ball milling revolutions in step (2) is 200 to 500R/min, and the ball milling time is 1 to 5 hours; the drying is carried out by keeping the temperature of 60-90 ℃ in an oven for 3-5h;
in the step (4), based on 100 percent of the initial slurry, the content of the organic carrier accounts for 10 to 20 weight percent, the content of the alumina powder accounts for 60 to 70 weight percent, and the balance is organic solvent;
the organic solvent is alcohol ester dodeca, terpineol or ethylene glycol monobutyl ether acetate;
the stirring is manual stirring or stirring by adopting a homogenizer;
and (5) rolling for 5-8 times by using a rolling mill, wherein the rolling mill is a zirconia three-roll rolling mill.
6. An alumina slurry obtained by the production method according to any one of claims 1 to 5.
7. A nitrogen-oxygen sensor, characterized in that the nitrogen-oxygen sensor uses the alumina slurry obtained by the preparation method of any one of claims 1 to 5 or the alumina slurry of claim 6.
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