CN113402285B - Low-temperature co-fired sintering agent for piezoelectric ceramics and preparation method thereof - Google Patents

Low-temperature co-fired sintering agent for piezoelectric ceramics and preparation method thereof Download PDF

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CN113402285B
CN113402285B CN202110574661.5A CN202110574661A CN113402285B CN 113402285 B CN113402285 B CN 113402285B CN 202110574661 A CN202110574661 A CN 202110574661A CN 113402285 B CN113402285 B CN 113402285B
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林秀娟
杨方慧
黄世峰
许新刚
冯云云
王超
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University of Jinan
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    • 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
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C04B2235/3248—Zirconates or hafnates, e.g. zircon
    • C04B2235/3249—Zirconates or hafnates, e.g. zircon containing also titanium oxide or titanates, e.g. lead zirconate titanate (PZT)
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/36—Glass starting materials for making ceramics, e.g. silica glass
    • C04B2235/365—Borosilicate glass
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment

Abstract

The invention discloses a piezoelectric ceramic low-temperature co-fired sintering agent and a preparation method and application thereof, wherein the piezoelectric ceramic low-temperature co-fired sintering agent comprises PZT ceramic powder, low-melting mixed glass powder and terpineol, the mass ratio of the PZT ceramic powder to the low-melting mixed glass powder is 1 to 5, the mass ratio of the PZT ceramic powder to the low-melting mixed glass powder to the terpineol is 2; the PZT ceramic powder, the low-melting mixed glass powder and the terpineol are mixed according to a proportion to prepare the piezoelectric ceramic low-temperature co-fired sintering agent which can be applied to the piezoelectric ceramic integrated sintering. The low-temperature co-fired sintering agent for the piezoelectric ceramics prepared by the invention has the same or similar thermal expansion coefficient with the piezoelectric ceramics, and can be matched with the structure, the mechanical property and the electrical property of the piezoelectric ceramics, so that the connected piezoelectric ceramics form an organic whole, the sintering temperature of the piezoelectric ceramics is effectively reduced, the volatilization of PbO is reduced, and the pollution to the environment is reduced on the basis of the original property of the piezoelectric ceramics.

Description

Low-temperature co-fired sintering agent for piezoelectric ceramics and preparation method thereof
Technical Field
The invention belongs to the technical field of low-temperature co-sintering materials, and particularly relates to a piezoelectric ceramic low-temperature co-sintering agent, and a preparation method and application thereof.
Background
Piezoelectric ceramics are an important branch of electronic information materials, and have wide application in the fields of aerospace, industry, medical treatment, civilian use and national defense, and the application range of the piezoelectric ceramics is gradually expanded along with the continuous progress of the piezoelectric ceramics materials and related technologies. PZT-based piezoelectric ceramics have the characteristics of high Curie temperature, high piezoelectric constant, excellent mechanical property, good stability and the like, and are in leading position in the field of piezoelectric ceramic materials at present. The sintering temperature of PZT is about 1200 ℃, lead oxide (volatilization temperature is 800 ℃) in the components is volatile at high temperature, so that the components deviate from the stoichiometric ratio, the piezoelectric property of the material is influenced, the environment is polluted, and the problem can be solved if the sintering can be carried out before PbO obviously volatilizes.
The low-temperature co-fired ceramic technology is a novel electronic packaging technology developed by the United states Huss company in 1982, is widely applied to various aspects such as base stations, automotive electronics, bluetooth, aerospace and the like at present, and has attracted people's attention in research, but has not been reported when being applied to integrated sintering among piezoelectric ceramic materials so that the piezoelectric ceramic forms an integrated material.
At present, low-temperature co-fired materials are classified into three categories: a glass ceramics system: such as Al 2 O 3 + A glass system having a low dielectric constant (ε r ≦ 10); amorphous glass system: fully mixing the oxides for forming the glass, and calcining at 800-950 ℃; glass + ceramic composite system: this is the most common LTCC material at present, i.e. low melting point glass phase is added to the ceramic, and the glass softens and the viscosity decreases during sintering, so that the sintering temperature can be reduced. In addition to the matrix material forming the glass or ceramic, some additives, such as sintering aid, etc., are usually added to the system to improve the devitrification ability, sintering property, electrical properties, etc. of the system.
Disclosure of Invention
The invention provides a low-temperature co-fired ceramic sintering agent and a preparation method and application thereof, aiming at the problems of high sintering temperature, poor electrical and mechanical properties and poor interface coupling property of a bonding agent for bonding and integrating ceramic materials in the prior art, wherein the piezoelectric ceramic low-temperature co-fired sintering agent prepared by the method has the same or similar thermal expansion coefficient with the piezoelectric ceramic materials, can realize integrated sintering, and simultaneously reduces the sintering temperature.
The invention is realized by the following technical scheme:
a piezoelectric ceramic low-temperature co-fired sintering agent comprises PZT ceramic powder, low-melting mixed glass powder and terpineol; the mass ratio of the PZT ceramic powder to the low-melting-point mixed glass powder is 1 to 5, and is 9 to 5; the mass ratio of the PZT ceramic powder to the low-melting mixed glass powder to the terpineol is 2.
Further, the low-melting-point mixed glass powder comprises the following components in parts by weight: siO 2 2 20~50%，Al 2 O 3 0~5.0%，B 2 O 3 15~30%,Na 2 O 1~10z%,K 2 O 0~2.0%,Li 2 O 1~5%,CaO0~5%,MgO 1~5%，ZnO 15~25%,ZrO 2 1~5%,TiO 2 0~2.0%,Bi 2 O 3 0~5.0%。
Go toThe low-melting-point mixed glass powder comprises the following components in parts by weight: siO 2 2 27.0%，Al 2 O 3 2.0%，B 2 O 3 30.0%，Na 2 O 5.0%，K 2 O 2.0%，LiO 2 3.0%，CaO 3.0%，MgO 1.0%，ZnO19.0%，ZrO 2 3.0%，Bi 2 O 3 5.0%
The method is further characterized in that the mass ratio of the PZT ceramic powder to the low-melting-point mixed glass powder is 1.
In the invention, the preparation method of the piezoelectric ceramic low-temperature co-fired sintering agent comprises the following steps: mixing PZT ceramic powder, low-melting mixed glass powder and terpineol in proportion to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
In the invention, the piezoelectric ceramic low-temperature co-fired sintering agent is applied to piezoelectric ceramic integrated sintering.
Furthermore, the sintering temperature of the piezoelectric ceramic low-temperature co-fired sintering agent during piezoelectric ceramic integrated sintering is 700 to 750 ℃.
The glass transition temperature of the low-melting-point glass powder is 450-500 ℃, the glass softening temperature range is 490-560 ℃, the melting temperature range is 540-660 ℃, the melt flow range is 700-750 ℃, and the thermal expansion coefficient is 5.5-8.4 x 10 in the temperature range of 30-400 DEG C -6 The low-melting-point glass powder has the same or similar thermal expansion coefficient with the piezoelectric ceramic material, and can realize integrated sintering.
Advantageous effects
The low-temperature co-fired sintering agent for the piezoelectric ceramics has the same or similar thermal expansion coefficient with the piezoelectric ceramics, can be matched with the structure, mechanical property and electrical property of the piezoelectric ceramics, enables the connected piezoelectric ceramics to form an organic whole, improves the electrical property and the mechanical property of the piezoelectric ceramics bonded by organic glue, and simultaneously introduces the low-temperature co-fired ceramic technology into the sintering of the piezoelectric ceramics, can effectively reduce the sintering temperature of the piezoelectric ceramics, reduce the volatilization of PbO in lead-based piezoelectric ceramics, avoid the deviation of the stoichiometric ratio of ceramic components, and reduce the pollution to the environment on the basis of ensuring the original good property of the piezoelectric ceramics.
Detailed Description
In order to make the technical solutions of the present invention better understood, the following description is provided clearly and completely, and other similar embodiments obtained by those skilled in the art without creative efforts shall fall within the protection scope of the present application based on the embodiments in the present application.
The parts described in the examples of the present invention are parts by weight.
Example 1
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 45.0%，B 2 O 3 15.0%，Na 2 O 6.0%，K 2 O 1.0%，LiO 2 3.0%，CaO1.0%，ZnO 2 4.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 90 parts of the low-melting-point mixed glass powder obtained in the step (1), 10 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 2
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 27.0%，Al 2 O 3 2.0%，B 2 O 3 30.0%，Na 2 O 5.0%，K 2 O 2.0%，LiO 2 3.0%，CaO 3.0%，MgO 1.0%，ZnO19.0%，ZrO 2 3.0%，Bi 2 O 3 5.0%；
(2) And (2) mixing 80 parts of the low-melting-point mixed glass powder in the step (1), 20 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 3
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 40.0%，Al 2 O 3 3.0%，B 2 O 3 18.0%，Na 2 O 10.0%，LiO 2 1.0%，ZnO 22.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 80 parts of the low-melting-point mixed glass powder in the step (1), 20 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 4
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 45.0%，B 2 O 3 15.0%，Na 2 O 6.0%，K 2 O 1.0%，LiO 2 3.0%，CaO1.0%，ZnO 2 4.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 70 parts of the low-melting-point mixed glass powder in the step (1), 30 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 5
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 27.0%，Al 2 O 3 2.0%， B 2 O 3 30.0%，Na 2 O 5.0%，K 2 O 2.0%，LiO 2 3.0%，CaO 3.0%，MgO 1.0%， ZnO19.0%， ZrO 2 3.0%，Bi 2 O 3 5.0%；
(2) And (2) mixing 60 parts of the low-melting-point mixed glass powder in the step (1), 40 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 6
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 40.0%，Al 2 O 3 3.0%， B 2 O 3 18.0%，Na 2 O 10.0%，LiO 2 1.0%，ZnO 22.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 50 parts of the low-melting-point mixed glass powder obtained in the step (1), 50 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 7
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 27.0%，Al 2 O 3 2.0%， B 2 O 3 30.0%，Na 2 O 5.0%，K 2 O 2.0%，LiO 2 3.0%，CaO 3.0%，MgO 1.0%， ZnO19.0%， ZrO 2 3.0%，Bi 2 O 3 5.0%；
(2) And (2) mixing 90 parts of the low-melting-point mixed glass powder in the step (1), 10 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 8
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 40.0%，Al 2 O 3 3.0%， B 2 O 3 18.0%，Na 2 O 10.0%，LiO 2 1.0%，ZnO 22.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 80 parts of the low-melting-point mixed glass powder in the step (1), 20 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 9
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 45.0%，B 2 O 3 15.0%，Na 2 O 6.0%，K 2 O 1.0%，LiO 2 3.0%，CaO 1.0%，ZnO 2 4.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 70 parts of the low-melting-point mixed glass powder in the step (1), 30 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 10
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 40.0%，Al 2 O 3 3.0%， B 2 O 3 18.0%，Na 2 O 10.0%，LiO 2 1.0%，ZnO 22.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 60 parts of the low-melting-point mixed glass powder in the step (1), 40 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Example 11
(1) The mixed glass powder with low melting point comprises the following components in percentage by weight: siO 2 2 45.0%，B 2 O 3 15.0%，Na 2 O 6.0%，K 2 O 1.0%，LiO 2 3.0%，CaO1.0%，ZnO 2 4.0%，ZrO 2 4.0%，TiO 2 2.0%；
(2) And (2) mixing 50 parts of the low-melting-point mixed glass powder in the step (1), 50 parts of PZT ceramic powder and 50 parts of terpineol to prepare the piezoelectric ceramic low-temperature co-fired sintering agent.
Performance test
(1) And (3) comparing and analyzing the thermal expansion coefficient and the thermal phase transition temperature of the mixed glass powder:
the thermal expansion coefficients and the thermal phase transition temperatures of the three groups of low-melting-point mixed glass powders in the steps (1) of the examples 1 to 3 are compared, and the results are shown in the following tables 1 and 2:
TABLE 1 thermal expansion coefficients (mum/DEG C) of three groups of low melting point mixed glass powders of examples 1 to 3 in different temperature ranges
Figure 135289DEST_PATH_IMAGE001
TABLE 2 examples 1 to 3 three groups of low melting point glass powder having a thermal transition temperature (. Degree. C.)
Figure 327236DEST_PATH_IMAGE002
As can be seen from table 1, the three melting point mixed glass powders in the embodiment of the present invention have the same or similar thermal expansion coefficients to the PZT piezoelectric ceramic material, and can achieve good matching with the PZT piezoelectric ceramic material; from table 2, it can be seen that the phase transition temperatures of the three melting point mixed glass powders in the embodiment of the present invention are set to 700 ℃ and 750 ℃ in order to ensure that the low temperature sintering agent can be completely melted and flows uniformly.
(2) And (3) testing electrical properties:
a2 mm flat PZT ceramic sample with the thickness of 4mm, 4mm and 2mm is prepared, the piezoelectric ceramic low-temperature co-fired sintering agents prepared in the examples 1 to 11 are bonded on one side, then sintering is carried out (wherein the sintering temperature of the piezoelectric ceramic low-temperature co-fired sintering agents of the examples 1 to 6 is 700 ℃, the sintering time is 2h, the sintering temperature of the piezoelectric ceramic low-temperature co-fired sintering agents of the examples 7 to 11 is 750 ℃, and the sintering time is 2 h), the sintered piezoelectric ceramic is subjected to high-voltage polarization treatment, the polarization temperature is 120 ℃, the piezoelectric ceramic is polarized for 15min according to the voltage of 3kV/mm, and the electrical and mechanical properties of the piezoelectric ceramic are tested. The piezoelectric strain constant and the relative dielectric constant were investigated by setting the epoxy resin composition as a comparison, and as a result, as shown in table 3 below, the electrical properties of the low-temperature sintering agent after sintering were excellent and much higher than those of the epoxy resin, as seen from table 3, among which the electrical properties of examples 3 and 7 were the best.
TABLE 3 comparison of the electrical properties of the low-temperature co-fired sintering agents for piezoelectric ceramics in examples 1 to 11 and epoxy resins
Figure 938346DEST_PATH_IMAGE003
(3) Mechanical property detection
The piezoelectric ceramic low-temperature co-firing sintering agent prepared in the example 3 and the example 7 with the best electrical property is selected as an integrated sintering material, the PZT piezoelectric ceramic with a rod-shaped structure is selected as a substrate, sintering is respectively carried out at 700 ℃ and 750 ℃ to realize integration, a three-point bending resistance test is carried out after sintering is finished, and an original ceramic substrate which is not subjected to secondary sintering is set as a blank sample group (PZT ceramic) and an epoxy resin bonding group as a reference to carry out mechanical property test.
Three-point bending is a loading mode for measuring bending strength, namely, a sample is arranged between two lower sticks and an upper stick, the upper stick is positioned between the lower sticks, and the upper and lower sticks move relatively to cause the sample to bend. The principle is that the load is monitored through a displacement-time relation graph during the test, the bending load is applied to a long strip sample with a rectangular cross section until the sample is broken, and the bending strength of the sample is calculated through the critical load, the span and the sample size when the sample is broken.
The specific experimental method is as follows, the ceramic-bending mechanical property test of stick bonding is carried out on the low-temperature sintering agent of the components according to the national standard (GB/T17671-1999), the beam speed of the experimental machine is 0.5mm/min, the sample size is 3mm, 4mm, 45mm, the chamfer angle is 45 degrees, each group of samples is not less than ten, and the average bending strength is calculated by mechanical comparison with the original ceramic matrix sample group and the epoxy resin bonding group which are not subjected to secondary sintering. The results of the average bending strength of each sample group are shown in table 4 below, and it can be seen from table 4 that the mechanical properties of PZT ceramics are the best, while example 3 has better electrical properties but poorer mechanical properties, and the low-temperature co-fired sintering agent for piezoelectric ceramics prepared in example 7 has not only good electrical properties but also excellent mechanical properties, which are obviously superior to the properties of epoxy resin.
TABLE 4 comparison of mechanical properties of PZT ceramics, low-temperature co-fired ceramic sintering agent and epoxy resin
Figure 72393DEST_PATH_IMAGE004
。

Claims (5)

1. A piezoelectric ceramic low-temperature co-firing sintering agent is characterized by comprising PZT ceramic powder, low-melting mixed glass powder and terpineol; the mass ratio of the PZT ceramic powder to the low-melting-point mixed glass powder is 1 to 5, and 9 to 5; the mass ratio of the PZT ceramic powder to the low-melting-point mixed glass powder to the terpineol is 2;
the low-melting-point mixed glass powder comprises the following components in parts by weight: siO 2 2 27.0%，Al 2 O 3 2.0%，B 2 O 3 30.0%，Na 2 O 5.0%，K 2 O 2.0%，LiO 2 3.0%，CaO 3.0%，MgO 1.0%，ZnO 19.0%，ZrO 2 3.0%，Bi 2 O 3 5.0%。
2. The low-temperature co-fired piezoelectric ceramic sintering agent according to claim 1, wherein the mass ratio of the PZT ceramic powder to the low-melting-point mixed glass powder is 1.
3. A method for preparing a low-temperature co-fired sintering agent for piezoelectric ceramics as defined in claim 1, characterized in that PZT ceramic powder, low-melting mixed glass powder and terpineol are mixed in proportion to prepare the low-temperature co-fired sintering agent for piezoelectric ceramics.
4. The use of the low-temperature co-fired sintering agent for piezoelectric ceramics according to claim 1 in the integrated sintering of piezoelectric ceramics.
5. The piezoelectric ceramic low-temperature co-fired sintering agent as claimed in claim 4, wherein the sintering temperature of the piezoelectric ceramic low-temperature co-fired sintering agent during piezoelectric ceramic integrated sintering is 700-750 ℃.
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