CN112390644B - Method for improving quality of MCT ceramic once ball-milling mixed material - Google Patents
Method for improving quality of MCT ceramic once ball-milling mixed material Download PDFInfo
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- CN112390644B CN112390644B CN202011317438.4A CN202011317438A CN112390644B CN 112390644 B CN112390644 B CN 112390644B CN 202011317438 A CN202011317438 A CN 202011317438A CN 112390644 B CN112390644 B CN 112390644B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/06—Selection or use of additives to aid disintegrating
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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Abstract
A method for improving the quality of MCT ceramic one-time ball milling mixed materials comprises the following specific process steps: preparing a citric acid solvent, adding the citric acid solvent, adding a strontium titanate modifier, adding a dispersing agent and an anti-settling agent, adding a magnesium oxide raw material, adding a titanium dioxide raw material, adding titanium dioxide powder, adding a calcium carbonate raw material, adding a certain amount of pure water, adjusting a ball mill to enter a ball milling working state, performing primary ball milling and mixing according to designed time and other process steps. The problems of continuity of existing MCT microwave dielectric ceramic powder, such as difficulty in controlling mixing technological conditions, incapability of fully dissolving raw materials in a solvent, slurry caking in a ball mill, extremely poor slurry dispersing effect, serious slurry caking, poor ball milling uniformity, reduction in production yield, increase in unqualified products, reduction in quality of the whole batch of products and the like, are solved. The method is widely applied to the manufacturing process of MCT-based microwave dielectric ceramics.
Description
Technical Field
The invention relates to the technical field of electronic components, in particular to a preparation method of MCT-based microwave dielectric ceramic.
Background
In the production technology of the existing ceramic powder, when the raw material is mixed and ground for one time, the feeding sequence is generally adopted and is as follows in sequence: raw materials, a dispersing agent, an additive and water; or raw materials, water, dispersants, additives. But for microwave dielectric ceramic MCT (MgTiO) 3 -CaTiO 3 ) Because the basic raw materials of MCT microwave dielectric ceramic are MgO, caO, tiO and other substances, whether the raw materials can be fully dissolved in the solvent in the ball milling process is greatly influenced by the factors of feeding sequence, time, speed and the like, if soThe mixing conditions cannot be strictly controlled, and the raw materials deviate from an optimized state which is difficult to control, so that whether the raw materials can be fully dissolved in a solvent or not is avoided, slurry caking is generated in a ball mill, the slurry dispersing effect is extremely poor, the slurry caking is serious, the ball milling uniformity is poor, the production qualification rate is reduced, and unqualified products are increased; reducing the quality of the whole batch of product.
Production line tests prove that a large amount of powder agglomerated hard blocks can be generated in the ball mill, and about 10 kg-30kg of agglomerated hard blocks can be estimated to be generated every 300kg of materials. The agglomeration is difficult to remove, the residue in the ball mill is difficult to clean manually, the raw materials of the product run off, the deviation between a production processing formula and a design formula is caused, the raw materials are not uniformly dispersed, finally, the dielectric property does not reach the standard, the quality of the product is influenced, and large-batch unqualified products are produced.
The cleaning equipment consumes a large amount of water, the equipment consumes a large amount of electricity during operation, and an operator needs about 4 hours to clean the equipment, so that a large amount of resources are wasted.
In addition, during manual cleaning: the slurry is caked, which easily causes the blockage of all pipelines in the next procedure, a large amount of slurry flows, and a large amount of time and a large amount of water resources are needed for dredging the pipelines. When the blockage is serious, the operation of the spray tower needs to be stopped, all equipment is shut down and production is stopped, a large amount of working time needs to be consumed additionally for maintenance, various resources such as water, electricity, gas, manpower and the like are wasted seriously, and the production cost is greatly increased.
Therefore, the invention is especially provided.
Disclosure of Invention
The purpose of the invention is: the method solves the problem of continuity that in the existing MCT microwave dielectric ceramic powder preparation process, the mixing process conditions are not easy to control, so that whether raw materials can not be fully dissolved in a solvent or not is caused, slurry caking is generated in a ball mill, the slurry dispersing effect is extremely poor, the slurry caking is serious, the ball milling uniformity is poor, the production yield is reduced, unqualified products are increased, the quality of the whole batch of products is reduced, and the like.
The invention provides a method for improving the quality of MCT ceramic one-time ball milling mixed materials, which is characterized in that the method utilizes the self chemical reaction of raw materials in a solution, the ball milling raw materials added in front and at the back are fully dissolved in the solution, the solubility of each raw material reaches a steady state balance point, the raw materials are fully fused during ball milling, slurry reaches an optimal state, the mixing is uniform, the slurry does not agglomerate, the ball milling process is stably completed, an ideal powder ball milling state is realized, and then the process can be carried out in the next manufacturing procedure.
The specific process steps are as follows:
1. preparing a citric acid solvent: pouring a certain amount of citric acid particles into a clean plastic bucket, adding hot pure water with a certain volume and temperature, adjusting the rotating speed of an electric stirrer according to requirements, and stirring according to a designed time to prepare the citric acid solvent with a set pH value. The solubility of the citric acid is increased along with the rise of the water temperature, and the citric acid and the pure water are better dissolved by the temperature rise and the stirring, so that the subsequent powder mixing is more favorable.
2. Adding a citric acid solvent: adding pure water with a set volume into a ball mill, and pouring the prepared quantitative citric acid solvent into the water solution of the ball mill. Can improve the solubility of the citric acid and ensure that the solvent is fully and uniformly distributed in the ball mill. Note: the citric acid can not be directly poured into the ball mill, so that the citric acid particles can not be dissolved in the solvent in time and are wrapped by other production powder.
3. The ball mill is started to rotate at a low speed.
4. Adding a modifier: adding quantitative strontium titanate powder while rotating for adjusting the dielectric property of MCT-based microwave dielectric ceramic (MCT ceramic);
5. adding an additive: while rotating, adding a certain amount of dispersant and anti-settling agent in turn. The formula of adding a small amount of small materials in the early stage is favorable for dissolving in a solvent, and if the small materials are added after a large amount of powder is added, the small materials are easily wrapped in other powder and are not fully dissolved, so that the function of adjusting the overall performance cannot be realized.
6. Adding magnesium oxide raw materials: adding the magnesium oxide powder while rotating. The magnesium oxide and water have weak reaction to generate magnesium hydroxide solution which is alkaline (MgO + H) in the whole environment 2 O=Mg(OH) 2 ) The alkaline environment is favorable for dissolving other raw materials.
7. Adding a titanium dioxide raw material: titanium dioxide powder is added while rotating. The solubility of titanium dioxide in water is lower than that in an alkaline environment, which facilitates dissolution (titanium dioxide solubility: alkaline solution > pure water).
8. Adding calcium carbonate raw materials: adding calcium carbonate powder while rotating. If calcium carbonate is added firstly, calcium ions can react with magnesium, titanium and manganese ions in the process of pouring materials to generate precipitates which are difficult to dissolve in water, and the production is influenced, so the calcium carbonate is added finally.
9. Adding a certain amount of pure water. In the process of adding water, the water pressure flushes agglomerated powder on the inner surface of the ball mill, which is beneficial to dissolving the powder in the solvent.
10. And adjusting the ball mill to enter a ball milling working state, and carrying out primary ball milling and mixing according to the designed time.
11. After the ball milling and mixing are finished, the subsequent manufacturing process can be carried out, and the needed MCT-based microwave dielectric ceramic (namely MCT ceramic) is obtained.
By adopting the method for improving the quality of the MCT ceramic once ball-milling mixed material, the slurry in the ball mill does not agglomerate after the MCT-based microwave dielectric ceramic once ball-milling mixed material is produced, the ball milling is uniform, the dispersibility is good, and the quality of the whole batch of products is improved; the cleaning ball milling tank saves a large amount of water, electricity and gas resources, reduces the labor intensity of workers, avoids the problems of cleaning and stopping equipment, increases the time for the equipment to be used for production, integrally promotes the product quality, improves the production efficiency and greatly reduces the production cost.
Drawings
FIG. 1 is a graph showing the results of a large amount of powder agglomerates generated after ball milling in the prior art.
FIG. 2 is a schematic diagram of the effect of no caking after the technical scheme of the invention is adopted.
Detailed Description
The specific embodiment of the method for improving the quality of the MCT ceramic primary ball milling mixed material in combination with the actual production of a production workshop is as follows:
1. controlling the environmental temperature of the ball milling workshop to be below 28 ℃ and controlling the humidity to be within 70%;
2. pouring 0.5 to 1kg of Citric Acid (CA) particles into a clean plastic bucket, adding 20 liters of hot pure water at 45 to 60 ℃, stirring for 3~5 minutes by using an electric stirrer at 200 to 500r/min, and pouring while stirring to fully dissolve the Citric Acid in the pure water in the bucket;
3. adding 160-180L of normal-temperature pure water into a ball mill;
4. pouring the prepared citric acid solvent into a ball mill;
5. adding 3 to 5kg of strontium titanate powder;
6. sequentially adding 1-2 kg of CE64 dispersing agent and 0.5-1kg of C42 anti-settling agent;
7. adding 100 to 110kg of magnesium oxide powder;
8. adding 180 to 190kg of titanium dioxide powder;
9. adding 14-15kg calcium carbonate powder;
10. adding 160-200L of pure water at normal temperature, washing the mixture in a citric acid bucket by using 20L of pure water, and adding washing water into a ball mill;
11. and starting the ball mill to perform ball milling.
The effect of this method is schematically shown in fig. 2, and the expected effect of the present invention is achieved.
The foregoing is a further detailed description of the invention in connection with preferred embodiments and is not intended to limit the invention to the precise form disclosed. It will be understood by those skilled in the art that various changes in detail may be effected therein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for improving the quality of MCT ceramic one-time ball milling mixed materials is characterized by comprising the following specific process steps:
(1) Preparing a citric acid solvent: pouring a certain amount of citric acid particles into a clean plastic barrel, adding hot pure water with certain volume and temperature, adjusting the rotating speed of an electric stirrer according to requirements, and stirring according to designed time to prepare a citric acid solvent with a set pH value;
(2) Adding a citric acid solvent: adding pure water with a set volume into a ball mill, and pouring the prepared quantitative citric acid solvent into the water solution of the ball mill;
(3) Starting the ball mill to rotate at a low speed;
(4) Adding a modifier: adding quantitative strontium titanate powder while rotating;
(5) Adding an additive: adding a certain amount of dispersing agent and anti-settling agent in turn while rotating;
(6) Adding a magnesium oxide raw material: adding magnesium oxide powder while rotating to make the citric acid solution after adding magnesium oxide powder alkaline;
(7) Adding a titanium dioxide raw material: adding titanium dioxide powder while rotating;
(8) Adding a calcium carbonate raw material: adding calcium carbonate powder while rotating;
(9) Adding a certain amount of pure water;
(10) And adjusting the ball mill to enter a ball milling working state, and carrying out primary ball milling and mixing according to the designed time.
2. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: and (2) before the step (1), controlling the ambient temperature of the ball milling workshop to be below 28 ℃ and controlling the humidity to be within 70%.
3. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: in the step (1), the citric acid is 0.5 to 1kg, the hot pure water is 20 liters, the water temperature is 45 to 60 ℃, the rotating speed of the electric stirrer is 200 to 500r/min, the stirring time is 3~5 minutes, and the stirring mode is pouring while stirring.
4. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: in the step (2), the pure water is 160 to 180 liters, and the water temperature is normal temperature.
5. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: in the step (4), the strontium titanate powder is 3 to 5kg.
6. The method for improving the quality of the MCT ceramic primary ball mill batch according to claim 1, wherein the method comprises the following steps: in the step (5), the type of the dispersing agent is CE64, the weight is 1-2kg, and the type of the anti-settling agent is C42, and the weight is 0.5-1kg.
7. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: in the step (6), the magnesium oxide powder is 100 to 110kg.
8. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: in the step (7), the titanium dioxide powder is 180 to 190kg.
9. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: in the step (8), 14-15kg of calcium carbonate powder is used.
10. The method for improving the quality of a primary ball-milled mixture of MCT ceramic as claimed in claim 1 wherein: and (9) in the step (9), the pure water is 160 to 200 liters, and the water temperature is normal temperature.
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| CN115445748B (en) * | 2022-09-28 | 2024-03-19 | 唐山贺祥智能科技股份有限公司 | Ceramic slurry ball milling grinding aid and ball milling process |
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