CN1785897A - Pressure proof strontium titanate base energy storage medium ceramic and its preparation method - Google Patents

Abstract

The present invention relates to a high pressure-resistant energy-storing medium ceramic and its preparation method. The chemical composition of said ceramic is Sr(Ti0.95 Zr0.05) O3+Xmol% CaTiSiO5, in which X is greater than O and less than or equal to 20. Its preparation method includes the following steps: adopting solid-phase method, using SrCO3 and TiO2 to synthesize SrTiO3; using SrCO3 and ZrO2 to synthesize SrZrO3; using CaCO3 SiO2 and TiO2 to synthesize CaTiSiO5 powder body; mixing materials according to the above-mentioned chemical composition formula; ball-grinding according to the ratio of material; ball: water=1:1:1-1.2, drying; adding polyvinyl alcohol solution as binding agent, granulating, sieving with 40 meshes, press-forming, slowly heating to 600-650deg.C to remove binding agent, sintering at 1260-1420deg.C, heat-insulating for 2-6hr, so as to obtain the invented product.

Description

A kind of pressure proof strontium titanate base energy storage medium ceramic and preparation method

Technical field

The present invention relates to a kind of pressure proof strontium titanate base energy storage medium ceramic and preparation method, specifically is a kind of with CaTiSiO ₅The SrTiO of doping vario-property ₃Base energy storage medium ceramic and preparation method.

Background technology

The pulse formation technology is the important topic in the research of high-voltage pulse power, and pulse-forming line is one of key factor of accelerator performance, and pulse compression commonly used forms structure coaxial configuration and slab construction.For adapting to the development that solid state pulse forms line, the direction of energy-accumulating medium forward low-resistance high current, miniaturization develops.Be applied to the energy-storing dielectric ceramic that solid state pulse forms line, should satisfy the requirement of following dielectric and voltage endurance: the relative permittivity ε that (1) is high _r(2) low dielectric loss tg δ, general requirement is tg δ≤1 * 10 under frequency of utilization ^-3(3) high disruptive strength E _bAt present, the research system of energy-storing dielectric ceramic has TiO ₂And BaTiO ₃TiO ₂Pottery has high disruptive strength, its E _b〉=35kv/mm, but TiO ₂The ceramic dielectric constant is not high, ε _r≈ 110; BaTiO ₃Pottery has high specific inductivity, its ε _r〉=1000, but BaTiO ₃The pottery disruptive strength is on the low side, E _b=5-8kv/mm, dielectric loss is bigger than normal, and has electrostriction phenomena.These drawbacks limit their application.SrTiO ₃The ceramic dielectric constant is higher relatively, ε _r≈ 250, and high-frequency loss is little, and electrostriction is little, but the low-frequency dielectric loss is bigger than normal, and disruptive strength E _bRelative TiO ₂Pottery still remains to be improved, and must improve to satisfy the requirement of energy-storing dielectric ceramic dielectric and voltage endurance.At present, do not see with CaTiSiO as yet ₅Doping improves SrTiO ₃The report of base ceramic dielectric and withstand voltage properties.

Summary of the invention

The purpose of this invention is to provide a kind of energy-storing dielectric ceramic, a kind of preparation method of this media ceramic is provided simultaneously with high-k, low-loss, higher disruptive strength.

The objective of the invention is to realize with following technical proposals:

A kind of pressure proof strontium titanate base energy storage medium ceramic, its chemical formula are Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, 0＜x≤20 wherein.

The preparation process of this energy-storing dielectric ceramic is:

1st, adopt analytically pure SrCO ₃And TiO ₂Raw material is pressed SrTiO ₃Chemistry adds and grinds the back oven dry behind the deionized water, at 4 hours synthetic SrTiO of 1150 ℃ of insulations than batching ₃Powder; Use analytically pure SrCO ₃And ZrO ₂Raw material is pressed SrZrO ₃Chemistry adds and grinds the back oven dry behind the deionized water, at 6 hours synthetic SrZrO of 1250 ℃ of insulations than batching ₃Powder; Adopt analytically pure CaCO ₃, SiO ₂And TiO ₂For raw material is pressed CaTiSiO ₅Chemistry adds and grinds the back oven dry behind the deionized water, at 2 hours synthetic CaTiSiO of 1050 ℃ of insulations than batching ₅Powder;

2nd, get the resulting SrTiO of step 1 ₃, SrZrO ₃And CaTiSiO ₅Powder is pressed Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, wherein 0＜x≤20 chemistry add the deionized water wet-milling and mix than batching, air atmosphere oven dry down;

3rd, add the polyvinyl alcohol water solution granulation at home and abroad to the resulting oven dry compound of step 2, compression moulding, sintering in the High Temperature Furnaces Heating Apparatus air atmosphere, making chemical formula is Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, the media ceramic of 0＜x≤20 wherein;

Wherein said polyvinyl alcohol water solution concentration is 0.5wt%～2.0wt%, and add-on is the 5wt%～10wt% of powder total amount; The pressure of described compression moulding is 100-120Mpa; Described sintering temperature is 1260-1420 ℃; Described sintering time is 2-6 hour.

At Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, wherein in the preparation of 0＜x≤20 energy-storing dielectric ceramics, our test-results is: CaTiSiO ₅Mix the firing temperature that can significantly reduce pottery, significantly improve the compressive strength of media ceramic simultaneously.When 0＜x≤2, firing temperature is 1350 ℃～1420 ℃, and the relative permittivity of media ceramic and dielectric loss change little, and dielectric strength enlarges markedly simultaneously; When 2＜x≤10, firing temperature is 1300 ℃～1350 ℃, and the relative permittivity of media ceramic descends obviously, and the dielectric loss of media ceramic will significantly increase dielectric strength decrease to some degree again simultaneously; When 10＜x≤20, firing temperature is 1260 ℃～1300 ℃, and CaTiSiO is arranged in the sintering process ₅Separate out, dielectric properties descend obviously.If polyvinyl alcohol (PVA) aqueous solution mass concentration that adds is less than 0.5%, sample is difficult to dry-pressing formed; If the PVA aqueous solution mass concentration that adds is greater than 2.0%, the media ceramic surface is easy to generate evil mind, and its withstand voltage properties is worsened; If soaking time is lower than 2 hours, sample media loss meeting is risen, if soaking time surpasses 6 hours, its withstand voltage properties can descend.

The present invention is by control CaTiSiO ₅Doping, overcome Sr (Ti _0.95Zr _0.05) O ₃The higher shortcoming of pottery firing temperature has obtained a kind of sintering at a lower temperature, the energy-storing dielectric ceramic with high-k, low-loss, higher disruptive strength.

Description of drawings

Fig. 1: the photo behind the silver-plated electrode of sample of embodiment 1-5 preparation.

Fig. 2: the XRD figure spectrum of the sample of embodiment 1-5 preparation.

Sample diameter is 20mm among Fig. 1, and thickness is 3mm, and the silver electrode diameter is 16mm.

Embodiment

The prescription of embodiment 1-5 is listed in table 1, and the performance of each embodiment sample is listed in table 2.

Table 1

Table 2

Test condition: show density applications Archimedes drainage and measure; Specific inductivity and dielectric loss are that frequency is that 1MHz measures down; Dielectric strength is being that medium is measured with insulating transformer oil.Probe temperature is room temperature.

Claims (2)

1, a kind of pressure proof strontium titanate base energy storage medium ceramic is characterized in that: its chemical formula is Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, 0＜x≤20 wherein.

2, a kind of method for preparing the described pressure proof strontium titanate base energy storage medium ceramic of claim 1 is characterized in that preparation process is:

1st, adopt analytically pure SrCO ₃And TiO ₂Raw material is pressed SrTiO ₃Chemistry adds and grinds the back oven dry behind the deionized water, at 4 hours synthetic SrTiO of 1150 ℃ of insulations than batching ₃Powder; Use analytically pure SrCO ₃And ZrO ₂Raw material is pressed SrZrO ₃Chemistry adds and grinds the back oven dry behind the deionized water, at 6 hours synthetic SrZrO of 1250 ℃ of insulations than batching ₃Powder; Adopt analytically pure CaCO ₃, SiO ₂And TiO ₂For raw material is pressed CaTiSiO ₅Chemistry adds and grinds the back oven dry behind the deionized water, at 2 hours synthetic CaTiSiO of 1050 ℃ of insulations than batching ₅Powder;

2nd, get the resulting SrTiO of step 1 ₃, SrZrO ₃And CaTiSiO ₅Powder is pressed Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, wherein 0＜x≤20 chemistry add the deionized water wet-milling and mix than batching, air atmosphere oven dry down;

3rd, add the polyvinyl alcohol water solution granulation at home and abroad to the resulting oven dry compound of step 2, compression moulding, sintering in the High Temperature Furnaces Heating Apparatus air atmosphere, making chemical formula is Sr (Ti _0.95Zr _0.05) O ₃+ xmol%CaTiSiO ₅, the media ceramic of 0＜x≤20 wherein;

Wherein said polyvinyl alcohol water solution concentration is 0.5wt%～2.0wt%, and add-on is the 5wt%～10wt% of powder total amount; The pressure of described compression moulding is 100-120Mpa; Described sintering temperature is 1260-1420 ℃; Described sintering time is 2-6 hour.

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