CN114217139A - Method for testing dielectric constant of barium titanate powder - Google Patents

Method for testing dielectric constant of barium titanate powder Download PDF

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CN114217139A
CN114217139A CN202111544348.3A CN202111544348A CN114217139A CN 114217139 A CN114217139 A CN 114217139A CN 202111544348 A CN202111544348 A CN 202111544348A CN 114217139 A CN114217139 A CN 114217139A
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barium titanate
ceramic chip
dielectric constant
silver
layer circular
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韩晖
胡石磊
涂志鑫
秦云峰
房满义
金彦章
邸道远
郭进
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Bengbu Zhongheng New Materials Scientific And Technological Co ltd
Anhui Zhongchuang Electronic Information Material Co ltd
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Bengbu Zhongheng New Materials Scientific And Technological Co ltd
Anhui Zhongchuang Electronic Information Material Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R27/00Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
    • G01R27/02Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
    • G01R27/26Measuring inductance or capacitance; Measuring quality factor, e.g. by using the resonance method; Measuring loss factor; Measuring dielectric constants ; Measuring impedance or related variables
    • G01R27/2617Measuring dielectric properties, e.g. constants
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R27/00Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
    • G01R27/02Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
    • G01R27/26Measuring inductance or capacitance; Measuring quality factor, e.g. by using the resonance method; Measuring loss factor; Measuring dielectric constants ; Measuring impedance or related variables
    • G01R27/2605Measuring capacitance

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Insulating Materials (AREA)
  • Ceramic Capacitors (AREA)

Abstract

The invention discloses a method for testing the dielectric constant of barium titanate powder, which comprises the steps of firstly adding 10-20% of adhesive by mass into barium titanate powder to be tested, preparing a barium titanate thin-layer circular ceramic chip with uniform size through a roller press, measuring the capacitance value of the circular ceramic chip by using a precise LCR digital bridge after the procedures of glue removal, silver coating and silver burning, and calculating the dielectric constant of the barium titanate powder through a formula according to the measured capacitance value and the thickness and the diameter of the circular ceramic chip. The method has strong operability and stable and reliable test results, and has important guiding significance in the aspects of factory detection and performance application of products.

Description

Method for testing dielectric constant of barium titanate powder
Technical Field
The invention belongs to the technical field of electronic materials, and particularly relates to a method for testing dielectric constant of barium titanate powder.
Background
Barium titanate is an inorganic substance with a chemical formula of BaTiO3It is a strong dielectric compound material, has high dielectric constant and low dielectric loss, is one of the most widely used materials in electronic ceramics, is mainly used for the preparation of various electronic components such as MLCC (chip multilayer ceramic capacitor), PTC thermistor and the like and the reinforcement of some composite materials, and is known as the pillar of the electronic ceramics industry.
The dielectric constant K is a main parameter reflecting the dielectric property or polarization property of the dielectric medium of the piezoelectric intelligent material under the action of an electrostatic field, and when the shape and the size of the piezoelectric intelligent material are fixed, the dielectric constant can be determined by measuring the inherent capacitance of the piezoelectric intelligent material.
When dielectric property test is carried out on barium titanate powder, the accuracy and stability of test results are extremely important. In the research, the regular wafer is found to have certain difficulty in preparation, the sample preparation process before the test is not explicitly described in the conventional test method, the test result has large fluctuation, and the test result is unreliable.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for testing the dielectric constant of barium titanate powder, which can accurately test the dielectric constant of the barium titanate powder, has strong operability and stable and reliable test result, and has important guiding significance in the aspects of factory detection and performance application of products.
In order to solve the technical problem, the invention provides a method for testing the dielectric constant of barium titanate powder, which comprises the following steps:
(1) preparing a barium titanate thin-layer circular ceramic chip:
adding 10-20% of adhesive in parts by mass into barium titanate powder to be detected, fully and uniformly stirring, slowly adding into an automatic roller press, rolling into barium titanate thin-layer raw ceramic cakes with consistent thickness, and then placing under a pressure plate of a sheet punching machine, and punching into a plurality of barium titanate thin-layer circular ceramic sheets with consistent sizes;
(2) rubber discharging:
placing the barium titanate thin-layer circular ceramic chip obtained in the step (1) on a clean and flat zirconia or alumina burning board, placing the ceramic chip and the burning board into a muffle furnace, and removing glue according to preset temperature rise and heat preservation parameters; after the front side binder removal, taking out the barium titanate thin-layer circular ceramic chip, turning over and binder removal for the back side;
(3) silver coating:
placing the barium titanate thin-layer circular ceramic chip subjected to glue discharging in the step (2) on a clean and flat zirconia or alumina burning board, and uniformly brushing silver paste on the front surface of the barium titanate thin-layer circular ceramic chip by using a fine brush;
(4) silver burning:
putting the barium titanate thin-layer circular ceramic chip coated with silver in the step (3) and the sintering plate into a muffle furnace, sintering silver according to preset temperature rise and heat preservation parameters, taking out the barium titanate thin-layer circular ceramic chip and the sintering plate after the front sintering silver is finished, and repeating the step (3) and the step (4) to sinter silver on the back;
(5) and (3) capacitance value measurement:
measuring the capacitance value C of the barium titanate thin-layer circular ceramic chip obtained after silver burning in the step (4) by using a precise LCR digital bridge;
(6) calculating the dielectric constant:
the thickness and diameter of the barium titanate thin-layer circular ceramic plate are measured by a vernier caliper, and according to the measured capacitance value C (nF) and the thickness h (mm) and diameter D (mm) of the barium titanate thin-layer circular ceramic plate, the formula K is equal to C multiplied by 144000 multiplied by h/D2The dielectric constant K of barium titanate was calculated.
Wherein the adhesive in the step (1) is prepared by compounding acrylic emulsion (PAA) and an alcamines plasticizer, and the decomposition temperature is less than 300 ℃; the preset temperature rising and heat preservation parameters in the step (4) are a temperature rising rate of 4-5 ℃/min, a heat preservation temperature of 800-900 ℃ and a heat preservation time of 1-3 h; the testing conditions of the precise LCR digital bridge in the step (5) are 1KHz, 1.0V and 25 ℃.
For simplicity, the method for testing the dielectric constant of barium titanate powder according to the present invention is simply referred to as the present method.
The method has strong operability, stable test result and good repeatability, and has strong guiding significance in the aspects of production quality control of barium titanate enterprises and application detection of downstream products.
Preferably, the barium titanate thin-layer circular ceramic chip in the step (1) is prepared by adopting a double-roller type roller press, wherein the roller is made of stainless steel and is subjected to surface polishing treatment; the gap between the two pairs of rollers is adjustable within the range of 0.5-2 mm, so that the surface of the porcelain cake is smooth and flat in the process of rolling and sample preparation, and materials cannot be polluted.
Preferably, the pressing plate of the sheet punching machine in the step (1) is circular, and the diameter of the pressing plate is 10-13 mm; the pressure plate is made of stainless steel, the surface of the pressure plate is polished, the surface of the ceramic chip is not polluted in the process of stamping and flaking, and the pressure plate is smooth and flat and is convenient for silver coating
Preferably, the temperature rising rate of the binder removal in the step (2) is 0.3-0.5 ℃/min, the heat preservation temperature is 300-400 ℃, the heat preservation time is 4-6 h, and the binder removal can be fully and completely ensured by controlling the temperature rising rate during calcination.
Preferably, the silver paste in the step (3) is a high-temperature sintered conductive silver paste, and the silver paste is brushed for 2-3 times in a unidirectional manner, wherein the thickness of the silver paste is 80-100 μm, so that the silver paste can be completely covered on the surface of the ceramic chip, and the ceramic chip is not exposed.
Preferably, in the step (4), before silver is fired, the silver layer adhered to the side surface of the barium titanate thin-layer circular tile is scraped off by a blade, so that the situation that silver paste is adhered to the side surface of the tile to form a passage to influence the test can be prevented.
By adopting the method, the fluctuation range of the test result of the dielectric constant of the same sample is less than 3 percent under the same test condition, and the method has obvious stability and repeatability.
Detailed Description
The invention will be further understood from the following examples, which are given by way of illustration and are not intended to be limiting.
Example 1
A method for testing the dielectric constant of barium titanate powder comprises the following steps:
(1) preparing a barium titanate thin-layer circular ceramic chip:
to 200g of barium titanate powder (tetragonal barium titanate, BaTiO) to be tested3Not less than 99.5%, crystal size 500 + -30 nm, Bet 2.1m2Adding 30g of adhesive into the mixture C/a (1.0105), stirring the mixture fully and uniformly, slowly adding the mixture into an automatic roller press, rolling the mixture into a barium titanate thin-layer raw material ceramic cake with the thickness of 1 +/-0.15 mm, and taking the barium titanate thin-layer raw material ceramic cake as qualified product with no color difference on the surface, uniform section and no obvious layering; then, placing the barium titanate thin layer raw material ceramic cake under a pressure plate of a sheet punching machine, and punching into 10 barium titanate thin layer circular ceramic sheets with the diameter of 11 +/-1 mm;
the water-soluble adhesive is prepared by compounding acrylic acid (PAA) emulsion and an alcamines plasticizer, and the decomposition temperature is less than 300 ℃;
the roller press is a double-roller type roller press, the rollers are made of stainless steel materials, and the surfaces of the rollers are polished; the gap between the two pairs of rollers is adjustable within the range of 0.5-2 mm;
the pressing disc of the sheet punching machine is circular, and the size is phi 10-phi 13 mm; the pressure plate is made of stainless steel and is subjected to surface polishing treatment.
(2) Rubber discharging:
placing the barium titanate thin-layer circular ceramic chip obtained in the step (1) on a clean and flat zirconia or alumina burning board, placing the ceramic chip and the burning board into a muffle furnace, and performing glue removal after heating to 350 ℃ at a heating rate of 0.5 ℃/min by heat preservation for 5 hours; and after the glue is discharged from the front side, taking out the barium titanate thin-layer circular ceramic chip, replacing the barium titanate thin-layer circular ceramic chip with the back side upward, and repeating the operation to discharge the glue from the back side.
(3) Silver coating:
and (3) placing the barium titanate thin-layer circular ceramic chip subjected to glue discharge in the step (2) on a clean and smooth zirconia or alumina burning board, uniformly coating silver paste on the front surface of the barium titanate thin-layer circular ceramic chip by using a fine brush, wherein the silver paste is high-temperature sintered conductive silver paste, and the silver paste is coated in a unidirectional manner for 2-3 times, and the thickness of the silver paste is 80-100 microns.
(4) Silver burning:
and (3) lightly scraping a silver layer adhered to the side surface of the barium titanate thin-layer circular ceramic chip coated with silver in the step (3) by using a blade, then putting the barium titanate thin-layer circular ceramic chip coated with silver and a setter plate into a muffle furnace, heating to 850 ℃ at a heating rate of 4.5 ℃/min, then carrying out heat preservation for 1h for silver burning, taking out the barium titanate thin-layer circular ceramic chip and the setter plate after the front silver burning is finished, and repeating the step (3) and the step (4) to carry out silver burning on the back surface.
(5) And (3) capacitance value measurement:
measuring the capacitance value C of the barium titanate thin-layer circular ceramic chip obtained after silver burning in the step (4) by using a precise LCR digital bridge under the test conditions of 1KHz, 1.0V and 25 ℃;
(6) calculating the dielectric constant:
the thickness and diameter of the barium titanate thin-layer circular ceramic plate are measured by a vernier caliper, and according to the measured capacitance value C (nF) and the thickness h (mm) and diameter D (mm) of the barium titanate thin-layer circular ceramic plate, the formula K is equal to C multiplied by 144000 multiplied by h/D2The dielectric constant K of barium titanate was calculated and the results are shown in Table 1.
Dielectric constant of barium titanate powder to be measured calculated in Table 1
C(nF) h(mm) D(mm) K And averageDeviation of value
1 2.86 1.1 11.39 3492.00 0.44%
2 2.83 1.13 11.43 3524.80 1.38%
3 2.87 1.09 11.4 3466.26 -0.30%
4 2.82 1.11 11.44 3444.15 -0.94%
5 2.84 1.11 11.42 3480.74 0.12%
6 2.86 1.08 11.43 3404.55 -2.08%
7 2.9 1.1 11.42 3522.26 1.31%
8 2.85 1.08 11.38 3422.52 -1.56%
9 2.84 1.1 11.4 3461.50 -0.44%
10 2.86 1.11 11.35 3548.62 2.07%
Mean value of 3476.34
As can be seen from Table 1, the dielectric constant K values of the barium titanate thin-layer circular ceramic tiles with the approximate sizes of 10 ceramic tiles are calculated to be between 3404.55 and 3548.62 under the same test conditions, and the fluctuation range is less than 3 percent.
Example 2
A method for testing the dielectric constant of barium titanate powder comprises the following steps:
(1) preparing a barium titanate thin-layer circular ceramic chip:
to 200g of barium titanate powder (tetragonal barium titanate, BaTiO) to be tested3Not less than 99.5%, crystal size 400 + -30 nm, Bet 2.9m240g of adhesive is added into the mixture C/a (1.0105), the mixture is fully stirred evenly, and then the mixture is slowly added into an automatic roller press to be rolled into a barium titanate thin-layer raw material ceramic cake with the thickness of 1 plus or minus 0.15mm, and the raw material ceramic cake is qualified in the aspects of no color difference on the surface, uniform section and no obvious layering; then, placing the barium titanate thin layer raw material ceramic cake under a pressure plate of a sheet punching machine, and punching into 10 barium titanate thin layer circular ceramic sheets with the diameter of 11 +/-1 mm;
the adhesive is prepared by compounding acrylic acid (PAA) emulsion and an alcamines plasticizer, and the decomposition temperature of the adhesive is less than 300 ℃;
the roller press is a double-roller type roller press, the rollers are made of stainless steel materials, and the surfaces of the rollers are polished; the gap between the two pairs of rollers is adjustable within the range of 0.5-2 mm;
the pressing disc of the sheet punching machine is circular, and the size is phi 10-phi 13 mm; the pressure plate is made of stainless steel and is subjected to surface polishing treatment.
(2) Rubber discharging:
placing the barium titanate thin-layer circular ceramic chip obtained in the step (1) on a clean and flat zirconia or alumina burning board, placing the ceramic chip and the burning board into a muffle furnace, and performing glue removal after heating to 300 ℃ at a heating rate of 0.3 ℃/min and preserving heat for 6 hours; and after the glue is discharged from the front side, taking out the barium titanate thin-layer circular ceramic chip, replacing the barium titanate thin-layer circular ceramic chip with the back side upward, and repeating the operation to discharge the glue from the back side.
(3) Silver coating:
and (3) placing the barium titanate thin-layer circular ceramic chip subjected to glue discharge in the step (2) on a clean and smooth zirconia or alumina burning board, uniformly coating silver paste on the front surface of the barium titanate thin-layer circular ceramic chip by using a fine brush, wherein the silver paste is high-temperature sintered conductive silver paste, and the silver paste is coated in a unidirectional manner for 2-3 times, and the thickness of the silver paste is 80-100 microns.
(4) Silver burning:
and (3) lightly scraping a silver layer adhered to the side surface of the barium titanate thin-layer circular ceramic chip coated with silver in the step (3) by using a blade, then placing the barium titanate thin-layer circular ceramic chip coated with silver and a setter plate into a muffle furnace, heating to 800 ℃ at a heating rate of 5 ℃/min, then carrying out heat preservation for 2 hours for silver burning, taking out the barium titanate thin-layer circular ceramic chip and the setter plate after the front silver burning is finished, and repeating the step (3) and the step (4) to carry out silver burning on the back surface.
(5) And (3) capacitance value measurement:
measuring the capacitance value C of the barium titanate thin-layer circular ceramic chip obtained after silver burning in the step (4) by using a precise LCR digital bridge under the test conditions of 1KHz, 1.0V and 25 ℃;
(6) calculating the dielectric constant:
the thickness and diameter of the barium titanate thin-layer circular ceramic plate are measured by a vernier caliper, and according to the measured capacitance value C (nF) and the thickness h (mm) and diameter D (mm) of the barium titanate thin-layer circular ceramic plate, the formula K is equal to C multiplied by 144000 multiplied by h/D2The dielectric constant K of barium titanate was calculated and the results are shown in Table 2.
Dielectric constant of barium titanate powder to be measured calculated in Table 2
C(nF) h(mm) D(mm) K Deviation from the mean value
1 2.53 1.11 11.44 3089.97 -0.49%
2 2.51 1.12 11.44 3093.16 -0.39%
3 2.49 1.14 11.47 3106.99 0.06%
4 2.46 1.12 11.34 3085.24 -0.64%
5 2.47 1.141 11.42 3109.08 0.12%
6 2.54 1.13 11.52 3114.37 0.29%
7 2.52 1.12 11.38 3138.31 1.06%
8 2.57 1.13 11.57 3123.97 0.60%
9 2.53 1.12 11.56 3053.41 -1.67%
10 2.48 1.14 11.39 3138.13 1.06%
Mean value of 3105.26
As can be seen from Table 2, the dielectric constant K value of barium titanate calculated from the above 10 thin-layer circular ceramic tiles of similar size is 3053.41-3138.31, and the fluctuation range is less than 3%
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.

Claims (10)

1. A method for testing the dielectric constant of barium titanate powder is characterized by comprising the following steps:
(1) preparing a barium titanate thin-layer circular ceramic chip:
adding 10-20% of adhesive in parts by mass into barium titanate powder to be detected, fully and uniformly stirring, slowly adding into an automatic roller press, rolling into barium titanate thin-layer raw ceramic cakes with consistent thickness, and then placing under a pressure plate of a sheet punching machine, and punching into a plurality of barium titanate thin-layer circular ceramic sheets with consistent sizes;
(2) rubber discharging:
placing the barium titanate thin-layer circular ceramic chip obtained in the step (1) on a clean and flat zirconia or alumina burning board, placing the ceramic chip and the burning board into a muffle furnace, and removing glue according to preset temperature rise and heat preservation parameters; after the front side binder removal, taking out the barium titanate thin-layer circular ceramic chip, turning over and binder removal for the back side;
(3) silver coating:
placing the barium titanate thin-layer circular ceramic chip subjected to glue discharging in the step (2) on a clean and flat zirconia or alumina burning board, and uniformly brushing silver paste on the front surface of the barium titanate thin-layer circular ceramic chip by using a fine brush;
(4) silver burning:
putting the barium titanate thin-layer circular ceramic chip coated with silver in the step (3) and the sintering plate into a muffle furnace, sintering silver according to preset temperature rise and heat preservation parameters, taking out the barium titanate thin-layer circular ceramic chip and the sintering plate after the front sintering silver is finished, and repeating the step (3) and the step (4) to sinter silver on the back;
(5) and (3) capacitance value measurement:
measuring the capacitance value C of the barium titanate thin-layer circular ceramic chip obtained after silver burning in the step (4) by using a precise LCR digital bridge;
(6) calculating the dielectric constant:
measuring the thickness and diameter of the barium titanate thin-layer circular ceramic chip by a vernier caliper, and according to the measured capacitance value C and the thickness h and diameter D of the barium titanate thin-layer circular ceramic chip, obtaining the barium titanate thin-layer circular ceramic chip by a formula K ═ Cx144000 xh/D2The dielectric constant K of barium titanate was calculated.
2. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: the water-soluble adhesive in the step (1) is prepared by compounding acrylic emulsion and an alcamines plasticizer, and the decomposition temperature is less than 300 ℃.
3. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: in the step (1), a double-roller type roller press is adopted for preparing the barium titanate thin-layer circular ceramic chip, rollers are made of stainless steel materials, and the surface of the rollers is polished; the gap between the two pairs of rollers is adjustable within the range of 0.5-2 mm.
4. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: the barium titanate thin-layer circular ceramic chip prepared in the step (1) is qualified by the fact that the surface has no chromatic aberration, the section is uniform, and no obvious layering exists.
5. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: the pressing plate of the sheet punching machine in the step (1) is circular, and the diameter of the pressing plate is 10-13 mm; the pressure plate is made of stainless steel and is subjected to surface polishing treatment.
6. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: in the step (2), the temperature rising rate of the discharged glue is 0.3-0.5 ℃/min, the heat preservation temperature is 300-400 ℃, and the heat preservation time is 4-6 h.
7. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: the silver paste in the step (3) is high-temperature sintering type conductive silver paste, and the silver paste is brushed for 2-3 times in a unidirectional manner, wherein the thickness of the silver paste is 80-100 mu m.
8. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: the preset heating and heat preservation parameters of silver firing in the step (4) are a heating rate of 4-5 ℃/min, a heat preservation temperature of 800-900 ℃ and a heat preservation time of 1-3 h.
9. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: and (4) scraping the silver layer adhered to the side surface of the barium titanate thin-layer circular ceramic chip by using a blade before silver burning.
10. The method for measuring dielectric constant of barium titanate powder according to claim 1, wherein: the testing conditions of the precise LCR digital bridge in the step (5) are 1KHz, 1.0V and 25 ℃.
CN202111544348.3A 2021-12-16 2021-12-16 Method for testing dielectric constant of barium titanate powder Pending CN114217139A (en)

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