CN115536377A - Black talc mineral microwave medium ceramic material and preparation method thereof - Google Patents
Black talc mineral microwave medium ceramic material and preparation method thereof Download PDFInfo
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Abstract
The application discloses a black talc mineral microwave dielectric ceramic material which is prepared by sintering the following raw materials in percentage by mass: 54-61% of the black talc ore powder, 33-40% of the MgO powder, 2-5% of MnCO 3 Powder and 1 to 4% of TiO 2 Powder, wherein the main material phase of the black talc mineral microwave medium ceramic material is Mg 2 SiO 4 A solid solution phase. The invention also discloses a preparation method of the black talc mineral microwave medium ceramic material, which comprises the step of carrying out wet ball milling on MgO powder and MnCO 3 Uniformly mixing the powder with the black talc powder pretreated in the step S1 in proportion, drying and calcining the mixture, and then carrying out wet ball milling on the calcined powder and TiO powder 2 And uniformly mixing the powder, the binder and the defoaming agent, drying, preparing a blank, and finally sintering. The invention adopts the components of compounding and ion modificationThe combined method realizes the preparation of the black talc mineral microwave dielectric ceramic material with high quality factor.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a black talc mineral microwave dielectric ceramic material and a preparation method thereof.
Background
The operating frequency required by 5G communication is higher and higher, the information transmission quantity is larger and larger from microwave to millimeter wave, and the requirements on microwave dielectric ceramic materials with low dielectric constant and low dielectric loss are stronger and stronger. Typical low dielectric constant systems today include Al 2 O 3 、Mg 2 SiO 4 、MgAl 2 O 4 And the relative dielectric constant is less than 10, the Q multiplied by f values are close to 60000GHz, and the temperature coefficient of the resonant frequency is close to zero, so that the application of devices such as microwave filters, antennas and the like can be well met.
In view of immeasurable prospects and benefits of the microwave dielectric ceramic material for 5G communication, the inventor adopts graphite tailings as a main raw material in previous researches to prepare the low-dielectric-constant microwave dielectric ceramic material (with the publication number of CN 113121214A) applicable to 5G communication, but due to more impurity types and contents of the tailings, the performance of the ceramic material cannot meet the application of high-quality microwave devices.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a black talc mineral microwave dielectric ceramic material and a preparation method thereof, provides a new preparation way for the microwave dielectric ceramic material for 5G mobile communication, and improves the quality factor of the material.
The technical scheme of the invention is as follows:
the application provides a black talc mineral microwave dielectric ceramic material which is prepared by sintering the following raw materials in percentage by mass: 54 to 61 percent of black talc ore powder, 33 to 40 percent of MgO powder and 2 to 5 percent of MnCO 3 Powder and 1-4% TiO 2 Powder, the main material phase of the black talc mineral microwave medium ceramic material is Mg 2 SiO 4 A solid solution phase.
Optionally, the black talc mineral microwave dielectric ceramic material has a dielectric constant of 6.78-7.40, a quality factor of 46356-71330 GHz, and a temperature coefficient of resonance frequency of-52 to-61 ppm/DEG C.
Optionally, the black talc ore powder is fine powder produced by concentrating black talc ore, the particle size of the fine powder is 38-48 mu m, and the chemical composition comprises SiO 2 、Al 2 O 3 、CaO、K 2 O、MgO、Fe 2 O 3 、Na 2 O and TiO 2 。
Further, the MgO powder and MnCO 3 Powder and TiO 2 The powders were all analytically pure.
The application also provides a preparation method of the black talc mineral microwave dielectric ceramic material, which comprises the following steps:
step S1, pretreating a black talc ore raw material to obtain black talc ore powder;
s2, performing wet ball milling on MgO powder and MnCO 3 Uniformly mixing the powder with the black talc powder pretreated in the step S1 in proportion;
s3, taking out the mixed powder obtained in the step S2, drying and calcining;
step S4, taking out the powder calcined in the step S3, and passing throughThe calcined powder and TiO are subjected to wet ball milling 2 Uniformly mixing the powder, the binder and the defoaming agent;
and S5, drying the mixture obtained in the step S4 to prepare a blank, and sintering the blank to obtain the ceramic material.
Optionally, the preprocessing process of step S1 is:
crushing and pulverizing 3-10 mm black talc ore particles to make the particle size less than 74 mu m, sieving to obtain powder with the particle size of 38-48 mu m, and finally calcining the powder in a high-temperature muffle furnace at the temperature of 700-900 ℃ for 4 hours.
Optionally, the specific steps of step S2 are:
firstly, adopting an ultrasonic dispersion machine to mix MgO and MnCO 3 And dispersing the powder in absolute ethyl alcohol to form a suspension for 10-30 min, mixing the suspension with the black talc powder pretreated in the step S1, and performing wet ball milling for 6-8 h at the rotating speed of 200-250 r/min.
Optionally, the specific steps in step S3 are:
and (3) taking out the powder obtained in the step (S2), carrying out heat treatment on the powder at 1100-1200 ℃, preserving heat for 2-3 h, and cooling along with the furnace after heat preservation is finished.
Optionally, the specific step of step S4 is:
uniformly mixing the binder, the defoaming agent and the deionized water by a stirring mode, stirring for 10-30 min, then mixing with the calcined powder obtained in the step S3, and performing wet ball milling for 4-8 h at the rotating speed of 250-300 r/min; the addition amount of the deionized water is 1-4 times, preferably 2 times of the mass of the powder, the addition amount of the binder is 0.15-0.3 wt% of the mass of the deionized water, and the addition amount of the defoaming agent is 0.3-0.6 wt% of the mass of the deionized water.
Optionally, the binder is polyvinyl alcohol and the defoamer is n-octanol.
Optionally, the specific step in step S5 is:
and (5) drying the mixture obtained in the step (S4), pressing the mixture into a blank, raising the temperature to 500-700 ℃ at the rate of raising the temperature to 5-8 ℃, discharging the glue for 2-4 h, then continuously raising the temperature to 1400-1600 ℃ at the rate of raising the temperature to 3-5 ℃, sintering for 6-8 h, and cooling along with the furnace after the sintering is finished.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) The application is based on the chemical composition of the black talc, and proper MgO is introduced to form Mg 2 SiO 4 Phase, so that the material has excellent microwave dielectric property, mnCO 3 And TiO 2 2 The small amount of doping reduces the dielectric loss of the material.
(2) Compared with the traditional ceramic solid phase preparation process, the preparation method has the advantages that the main material and the modifier are uniformly mixed through ultrasonic dispersion in advance; and a binder and a defoaming agent are introduced in the secondary ball milling, so that the quality of the ceramic slurry is improved, and a powder granulation process is avoided. The finally sintered ceramic particles are closely packed, the porosity is low, and the dielectric loss is lower.
(3) The proportion of the black talc ore in the formula is close to sixty percent, so that the raw material cost is greatly reduced, and the practical application of the black talc mineral microwave dielectric ceramic material is met.
Drawings
FIG. 1 is an XRD spectrum of a black talc ore powder raw material;
FIG. 2 is an XRD spectrum of a black talc mineral microwave dielectric ceramic material prepared in example 3 of the present invention;
FIG. 3 is an SEM image of a black talc mineral microwave dielectric ceramic material prepared in example 3 of the present invention;
FIG. 4 is an SEM image of a microwave dielectric ceramic material prepared in comparative example 1 of the present invention.
Detailed Description
Black talc is a layered magnesium-rich silicate, the main mineral is talc, and the secondary minerals are quartz and muscovite, which has wider application in the ceramic industry field, but the related field still has low added value and the technical threshold is relatively low. Therefore, the search for the high value-added application field of black talc in the ceramic industry is a problem to be solved urgently at present. The black talc contains more organic carbon with high dispersibility, has no stable performance of talc, but has a composition different from that of white talc after calcinationSmall, exhibiting MgSiO 3 、SiO 2 Two phases with low impurity content, and the composition of the phase and MgAl with low dielectric constant 2 O 4 The system is very close, can be regulated and controlled by adding sufficient Mg components, has low impurity content, is favorable for improving the microwave dielectric property, and further improves the application potential of the black talc-based microwave dielectric material.
The invention is further described with reference to the following figures and examples:
FIG. 1 is an XRD pattern of a black talc ore powder raw material. Referring to FIG. 1, the chemical components of the powdered source of black talc include SiO 2 、Al 2 O 3 、CaO、K 2 O、MgO、Fe 2 O 3 、Na 2 O and TiO 2 And the mineral phase consists of talc and quartz.
Example 1
S1: pulverizing black talc ore particles of 3-10mm by a jaw crusher to enable the particle size of the black talc ore particles to be smaller than 74 mu m, obtaining powder of 38-48 mu m by a mechanical screening method, and finally calcining the powder in a high-temperature muffle furnace for 4 hours at 700 ℃;
s2: 13.2g of analytically pure MgO powder and analytically pure MnCO powder are weighed 3 0.8g of powder, pouring the two kinds of powder into 80g of absolute ethyl alcohol, performing ultrasonic dispersion for 10min to form a suspension, then weighing 24.4g of pretreated black talc powder, mixing the suspension and the black talc powder, and performing wet ball milling for 6h at the rotating speed of 200r/min;
s3: taking out the mixed powder after ball milling, drying, placing in a muffle furnace for heat treatment at 1100 ℃, preserving heat for 2 hours, and cooling along with the furnace after heat preservation;
s4: analytically pure TiO is stirred by hand 2 1.6g of powder, 0.12g of polyvinyl alcohol, 0.24g of analytically pure octanol liquid and 80g of deionized water are uniformly mixed, stirred for 10min, then mixed with the powder calcined in the step S3, and subjected to wet ball milling for 4h at the rotating speed of 250r/min;
s5: and (4) drying the mixture obtained in the step (S4), putting the dried powder into a metal mold for cold press molding, putting the molded block into a high-temperature furnace, raising the temperature to 500 ℃ at the rate of 5 ℃ for binder removal for 2h, then continuously raising the temperature to 1400 ℃ at the rate of 3 ℃ for sintering for 6h, and cooling along with the furnace after sintering.
The microwave dielectric properties of the black talc mineral microwave dielectric ceramic material prepared in example 1 are measured as follows: dielectric constant ε r =6.78, quality factor Q × f =46356GHz, temperature coefficient of resonance frequency τ f = -61ppm/℃。
Example 2
S1: pulverizing black talc ore particles of 3-10mm by a jaw crusher to enable the particle size of the black talc ore particles to be smaller than 74 mu m, obtaining powder of 38-48 mu m by a mechanical screening method, and finally calcining the powder in a high-temperature muffle furnace for 4 hours at 800 ℃;
s2: weighing 14.4g of analytically pure MgO powder and 14.4g of analytically pure MnCO 3 1.2g of powder, pouring the two kinds of powder into 80g of absolute ethyl alcohol, performing ultrasonic dispersion for 20min to form a suspension, then weighing 23.6g of pretreated black talc powder, mixing the suspension and the black talc powder, and performing wet ball milling for 7h at the rotating speed of 220r/min;
s3: taking out the mixed powder after ball milling, drying, placing in a muffle furnace for heat treatment at 1150 ℃, preserving heat for 2.5h, and cooling along with the furnace after finishing the heat preservation;
s4: analytically pure TiO is stirred by hand 2 Uniformly mixing 0.8g of powder, 0.16g of polyvinyl alcohol, 0.32g of analytically pure octanol liquid and 80g of deionized water, stirring for 20min, mixing with the powder calcined in the step S3, and performing wet ball milling for 6h at the rotating speed of 270r/min;
s5: and (4) drying the mixture obtained in the step (S4), putting the dried powder into a metal die for cold press molding, putting the molded block into a high-temperature furnace, raising the temperature to 600 ℃ at the heating rate of 6 ℃ for 3 hours for binder removal, then continuously raising the temperature to 1450 ℃ at the heating rate of 4 ℃ for sintering for 7 hours, and cooling along with the furnace after sintering.
The microwave dielectric properties of the black talc mineral microwave dielectric ceramic material prepared in example 2 are measured as follows: dielectric constant ε r =6.94, quality factor Q × f =62563GHz, temperature coefficient of resonance frequency τ f = -52ppm/℃。
Example 3
S1: pulverizing black talc ore particles of 3-10mm by a jaw crusher to enable the particle size of the black talc ore particles to be smaller than 74 mu m, obtaining powder of 38-48 mu m by a mechanical screening method, and finally calcining the powder in a high-temperature muffle furnace for 4 hours at 800 ℃;
s2: weighing 14.8g of analytically pure MgO powder and analytically pure MnCO 3 1.6g of powder, pouring the two kinds of powder into 80g of absolute ethyl alcohol, performing ultrasonic dispersion for 20min to form a suspension, then weighing 22.4g of pretreated black talc powder, mixing the suspension with the black talc powder, and performing wet ball milling for 8h at the rotation speed of 200r/min;
s3: taking out the mixed powder after ball milling, drying, placing in a muffle furnace for heat treatment at 1100 ℃, preserving heat for 2 hours, and cooling along with the furnace after heat preservation;
s4: analytically pure TiO is stirred by hand 2 1.2g of powder, 0.2g of polyvinyl alcohol, 0.4g of analytically pure octanol liquid and 80g of deionized water are uniformly mixed, stirred for 20min, then mixed with the powder calcined in the step S3, and subjected to wet ball milling for 8h at the rotating speed of 300r/min;
s5: and (5) drying the mixture obtained in the step (S4), putting the dried powder into a metal mold for cold press molding, putting the molded block into a high-temperature furnace, heating to 700 ℃ at a heating rate of 7 ℃ for binder removal for 2h, then continuously heating to 1550 ℃ at a heating rate of 3 ℃ for sintering for 8h, and cooling along with the furnace after sintering.
The microwave dielectric properties of the black talc mineral microwave dielectric ceramic material prepared in example 1 are measured as follows: dielectric constant ε r =6.91, quality factor Q × f =71330GHz, temperature coefficient of resonance frequency τ f = -54ppm/℃。
Example 4
S1: pulverizing black talc ore particles of 3-10mm by a jaw crusher to enable the particle size of the black talc ore particles to be smaller than 74 mu m, obtaining powder of 38-48 mu m by a mechanical screening method, and finally calcining the powder in a high-temperature muffle furnace for 4 hours at 900 ℃;
s2: weighing 16.0g of analytically pure MgO powder and analytically pure MnCO 3 2.0g of powder, pouring the two powders into 80g of absolute ethyl alcohol, carrying out ultrasonic dispersion for 30min to form a suspension, then weighing 21.6g of pretreated black talc powder,mixing the suspension with black talc powder, and performing wet ball milling for 8 hours at the rotating speed of 250r/min;
s3: taking out the mixed powder after ball milling, drying, placing in a muffle furnace for heat treatment at 1200 ℃, preserving heat for 3 hours, and cooling along with the furnace after heat preservation;
s4: analytically pure TiO is stirred by hand 2 Uniformly mixing 0.4g of powder, 0.24g of polyvinyl alcohol, 0.48g of analytically pure octanol liquid and 80g of deionized water, stirring for 30min, mixing with the powder calcined in the step S3, and performing wet ball milling for 8h at the rotating speed of 300r/min;
s5: and (4) drying the mixture obtained in the step (S4), putting the dried powder into a metal mold for cold press molding, putting the molded block into a high-temperature furnace, raising the temperature to 700 ℃ at the heating rate of 8 ℃ for binder removal for 4h, then continuously raising the temperature to 1600 ℃ at the heating rate of 5 ℃ for sintering for 8h, and cooling along with the furnace after sintering.
The microwave dielectric properties of the black talc mineral microwave dielectric ceramic material prepared in example 1 are measured as follows: dielectric constant ε r =7.40, quality factor Q × f =44461GHz, resonant frequency temperature coefficient τ f = -56ppm/℃。
Comparative example 1
S1: pulverizing black talc ore particles of 3-10mm by a jaw crusher to enable the particle size of the black talc ore particles to be smaller than 74 mu m, obtaining powder of 38-48 mu m by a mechanical screening method, and finally calcining the powder in a high-temperature muffle furnace for 4 hours at 800 ℃;
s2: weighing 22.4g of pretreated black talc powder, 14.8g of analytically pure MgO powder and analytically pure MnCO 3 1.6g of powder, pouring all the powder into 80g of absolute ethyl alcohol, and then carrying out wet ball milling for 8 hours at the rotating speed of 200r/min;
s3: taking out the mixed powder subjected to ball milling, drying, placing in a muffle furnace for heat treatment at 1100 ℃, preserving heat for 2 hours, and cooling along with the furnace after the heat preservation is finished;
s4: mixing the calcined powder obtained in the step S3 with analytically pure TiO 2 Mixing 1.2g of powder and 80g of deionized water, and performing wet ball milling for 8 hours at the rotating speed of 300r/min;
s5: and (5) drying the mixture obtained in the step (S4), adding 0.2g of polyvinyl alcohol into the dried powder for granulation, then placing the powder into a metal mold for cold press molding, placing the molded block into a high-temperature furnace, raising the temperature to 700 ℃ at a heating rate of 7 ℃ for binder removal for 2 hours, then continuously raising the temperature to 1550 ℃ at a heating rate of 3 ℃ for sintering for 8 hours, and cooling along with the furnace after sintering.
Through measurement, the microwave dielectric properties of the black talc mineral microwave dielectric ceramic material prepared in the comparative example 1 are as follows: dielectric constant ε r =6.88, quality factor Q × f =52348GHz, temperature coefficient of resonance frequency τ f = -56ppm/℃。
Comparative example 2
S1: pulverizing black talc ore particles of 3-10mm by using a jaw crusher to enable the particle size of the black talc ore particles to be smaller than 74 micrometers, obtaining powder of 38-48 micrometers in particle size by using a mechanical screening method, and finally calcining the powder in a high-temperature muffle furnace for 4 hours at 900 ℃;
s2: 21.6g of pretreated black talc powder, 16.0g of analytically pure MgO powder and analytically pure MnCO are weighed 3 2.0g of powder, pouring all the powder into 80g of absolute ethyl alcohol, and then carrying out wet ball milling for 8 hours at the rotating speed of 200r/min;
s3: taking out the mixed powder after ball milling, drying, placing in a muffle furnace for heat treatment at 1200 ℃, preserving heat for 3 hours, and cooling along with the furnace after heat preservation;
s4: mixing the calcined powder obtained in the step S3 with analytically pure TiO 2 Mixing 0.4g of powder and 80g of deionized water, and performing wet ball milling for 8 hours at the rotating speed of 300r/min;
s5: and (4) drying the mixture obtained in the step (S4), adding 0.24g of polyvinyl alcohol into the dried powder for granulation, putting the dried powder into a metal mold for cold press molding, putting the molded block into a high-temperature furnace, raising the temperature to 700 ℃ at the heating rate of 8 ℃ for glue removal for 4h, then continuously raising the temperature to 1600 ℃ at the heating rate of 5 ℃ for sintering for 8h, and cooling along with the furnace after sintering.
Through measurement, the microwave dielectric properties of the black talc mineral microwave dielectric ceramic material prepared in the comparative example 2 are as follows: dielectric constant ε r =7.46, quality factor Q × f =27653GHz, temperature coefficient of resonance frequency τ f = -58ppm/℃。
Comparative example 3
S1: firstly, crushing graphite tailings into particles with the particle size of 3-10mm, further finely grinding to ensure that the particle size is smaller than 200 mu m, then obtaining tailing powder with the particle size of 45-75 mu m by a mechanical screening method, and finally dehydrating for 4 hours in an oven at the temperature of 120 ℃;
s2: 27.6g of pretreated graphite tailing powder and analytically pure Al are weighed 2 O 3 12g of powder, analytically pure BaCO 3 Powder 9g and analytically pure SrCO 3 Grinding 9g of powder by a mortar for 30min, and then tumbling for 6h by a dry method at the rotating speed of 150r/min;
s3: taking out the mixed powder after the barreling, placing the mixed powder in a muffle furnace for heat treatment at 950 ℃, preserving heat for 1.5h, and cooling along with the furnace after the heat preservation is finished;
s4: firstly, 2.4g of TiO is dispersed by an ultrasonic disperser 2 Dispersing the powder in 4.8g of absolute ethyl alcohol to form slurry, wherein the dispersion time is 5min, then pouring the calcined mixed powder into the slurry, and carrying out wet ball milling for 10h at the rotating speed of 300r/min;
s5: and (3) drying the mixture obtained in the step (S4), adding a binder accounting for 3wt% of the powder into the dried powder for granulation, then placing the powder into a metal die for cold press molding, placing the molded block into a high-temperature furnace for sintering at 1250 ℃ for 5 hours, cooling to 775 ℃ at a cooling rate of 1.5 ℃/min after sintering, and then cooling along with the furnace.
Through measurement, the microwave dielectric property of the graphite tailing-based microwave dielectric ceramic material prepared in the embodiment 3 is as follows: dielectric constant ε r =7.2, quality factor Q × f =34160GHz, temperature coefficient of resonance frequency τ f = 5ppm/℃。
In the embodiments 3 and 4, the raw material pre-dispersion is introduced on the basis of the traditional solid phase method, and the binder, the defoaming agent and other processes are introduced in the secondary ball milling, so that compared with the comparative examples 1 and 2, the prepared microwave dielectric ceramic material has a higher quality factor Qxf value and correspondingly lower dielectric loss.
FIG. 2 is an XRD spectrum of a black talc mineral microwave dielectric ceramic material prepared in example 3 of the present invention; FIG. 3 is an SEM image of a black talc mineral microwave dielectric ceramic material prepared in example 3 of the present invention. Referring to FIGS. 2 and 3, the method adopted in example 3 of the present applicationThe microwave dielectric ceramic material prepared by the preparation method has the advantages of close packing of ceramic particles and low porosity. FIG. 4 is an SEM image of a microwave dielectric ceramic material prepared in comparative example 1 of the present invention. Referring to fig. 4, the microwave dielectric ceramic material prepared in comparative example 1 by the conventional process has loose particles and more pores. Also, the quality factor of the black talc mineral microwave dielectric ceramic material prepared in examples 1 to 4Q×fThe values are all higher than in comparative example 3.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The black talc mineral microwave dielectric ceramic material is characterized by being prepared by sintering the following raw materials in percentage by mass: 54 to 61 percent of black talc ore powder, 33 to 40 percent of MgO powder and 2 to 5 percent of MnCO 3 Powder and 1-4% TiO 2 Powder, the main material phase of the black talc mineral microwave medium ceramic material is Mg 2 SiO 4 A solid solution phase.
2. The black talc mineral microwave dielectric ceramic material as claimed in claim 1, wherein said black talc mineral microwave dielectric ceramic material has dielectric constant of 6.78-7.40, quality factor of 46356-71330 GHz, and temperature coefficient of resonance frequency of-52 to-61 ppm/° C.
3. The black talc mineral microwave dielectric ceramic material as claimed in claim 1, wherein said black talc ore powder is fine particle powder produced by black talc ore concentration, particle size is in the range of 38-48 μm, chemical composition includes SiO 2 、Al 2 O 3 、CaO、K 2 O、MgO、Fe 2 O 3 、Na 2 O and TiO 2 。
4. A method for preparing a black talc mineral microwave dielectric ceramic material according to any one of claims 1 to 3, characterized by comprising the steps of:
step S1, pretreating a black talc ore raw material to obtain black talc ore powder;
s2, performing wet ball milling on MgO powder and MnCO 3 Uniformly mixing the powder with the black talc powder pretreated in the step S1 in proportion;
s3, taking out the mixed powder obtained in the step S2, drying and calcining;
s4, taking out the calcined powder in the step S3, and then carrying out wet ball milling on the calcined powder and TiO 2 Uniformly mixing the powder, the binder and the defoaming agent;
and S5, drying the mixture obtained in the step S4 to prepare a blank, and sintering the blank to obtain the ceramic material.
5. The method for preparing black talc mineral microwave dielectric ceramic material according to claim 4, wherein said pretreatment process of step S1 is:
crushing and pulverizing 3-10 mm black talc ore particles to make the particle size less than 74 mu m, sieving to obtain powder with the particle size of 38-48 mu m, and finally calcining the powder in a high-temperature muffle furnace at the temperature of 700-900 ℃ for 4 hours.
6. The method for preparing the black talc mineral microwave dielectric ceramic material as claimed in claim 4, wherein said step S2 is specifically the steps of:
firstly, adopting an ultrasonic dispersion machine to mix MgO and MnCO 3 And dispersing the powder in absolute ethyl alcohol to form a suspension for 10-30 min, mixing the suspension with the black talc powder pretreated in the step S1, and performing wet ball milling for 6-8 h at the rotating speed of 200-250 r/min.
7. The method for preparing black talc mineral microwave dielectric ceramic material according to claim 4, wherein said step S3 is specific step:
and (3) taking out the powder obtained in the step (S2), carrying out heat treatment on the powder at 1100-1200 ℃, preserving heat for 2-3 h, and cooling along with the furnace after heat preservation is finished.
8. The method for preparing black talc mineral microwave dielectric ceramic material according to claim 4, wherein said step S4 is specific steps:
uniformly mixing the binder, the defoaming agent and the deionized water by a stirring mode, stirring for 10-30 min, then mixing with the calcined powder obtained in the step S3, and performing wet ball milling for 4-8 h at the rotating speed of 250-300 r/min; the additive amount of the deionized water is 1-4 times of the mass of the powder, the additive amount of the binder is 0.15-0.3 wt% of the mass of the deionized water, and the additive amount of the defoaming agent is 0.3-0.6 wt% of the mass of the deionized water.
9. The method of claim 8, wherein the binder is polyvinyl alcohol and the defoamer is n-octanol.
10. A method for preparing a black talc mineral microwave dielectric ceramic material according to any one of claims 4 to 9, wherein said specific step in step S5 is:
and (4) drying the mixture obtained in the step (S4), pressing the mixture into a blank, raising the temperature to 500-700 ℃ at the rate of temperature rise of 5-8 ℃ for discharging glue for 2-4 h, then continuously raising the temperature to 1400-1600 ℃ at the rate of temperature rise of 3-5 ℃ for sintering for 6-8 h, and cooling along with the furnace after sintering.
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| WO2024114334A1 (en) * | 2022-11-29 | 2024-06-06 | 苏州中材非金属矿工业设计研究院有限公司 | Black talc mineral microwave dielectric ceramic material and preparation method therefor |
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