CN1927764A - Seepage flow type silver/strontium barium titanate/nonex composite material and manufacture method - Google Patents
Seepage flow type silver/strontium barium titanate/nonex composite material and manufacture method Download PDFInfo
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- CN1927764A CN1927764A CN200610053707.4A CN200610053707A CN1927764A CN 1927764 A CN1927764 A CN 1927764A CN 200610053707 A CN200610053707 A CN 200610053707A CN 1927764 A CN1927764 A CN 1927764A
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- barium titanate
- strontium
- pbo
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 20
- 229910002113 barium titanate Inorganic materials 0.000 title claims description 37
- 239000004332 silver Substances 0.000 title claims description 19
- 239000002131 composite material Substances 0.000 title abstract description 5
- 238000000034 method Methods 0.000 title description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title description 2
- 238000004519 manufacturing process Methods 0.000 title 1
- 229910052712 strontium Inorganic materials 0.000 title 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims description 39
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 24
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 claims description 20
- 238000000748 compression moulding Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 4
- 101000635799 Homo sapiens Run domain Beclin-1-interacting and cysteine-rich domain-containing protein Proteins 0.000 abstract 2
- 102100030852 Run domain Beclin-1-interacting and cysteine-rich domain-containing protein Human genes 0.000 abstract 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000004020 conductor Substances 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The present invention discloses seepage flowing Ag/baron strontium titanate/nonex composite material comprising substrate material Ba0.8Sr0.2TiO3/PbO-B2O3 in 70-99 vol% and Ag in 1-30 vol%. The preparation process of the composite material includes the following steps: 1. mixing baron strontium titanate powder and nonex powder based on the stoichiometric ratio of Ba0.8Sr0.2TiO3/PbO-B2O3 to obtain substrate powder; 2. mixing the substrate powder and Ag powder in the required ratio, grinding and pressing to form; and 3. sintering the formed material at 800-900 deg.c. The composite material has very high dielectric constant, relatively small dielectric loss and relatively high frequency stability, temperature stability of dielectric constant, and thus excellent application foreground.
Description
Technical field
The present invention relates to a kind of seepage flow type silver/strontium-barium titanate/nonex matrix material and preparation method thereof, belong to the dielectric ceramic technical field.
Background technology
In recent years, because strontium-barium titanate (BST) has superior physicals, for example loss is low, and dielectric relaxation time is short etc., thereby is widely regarded as and is used to make the microwave acousticresonance device, pyroelectric sensor, the ideal material of phase converter and electrical condenser.But when strontium-barium titanate (BST) was in the solid state sintering, the sintering temperature of pottery was approximately 1400 ℃, and this has limited its application on integrated circuit processing technique to a great extent.As everyone knows, adopt the method that adds glassy phase at strontium-barium titanate (BST), can form nucleocapsid structure.This method not only can make it become pottery and densification at lower sintering temperature, and can improve the dielectric properties as some aspect of temperature-stable electrical condenser.For strontium-barium titanate (BST)/glassy phase material, research is less at present, people such as Wu Rong in 2006 at Material Chemistry and Physics (Wu Rong, Du Piyi, et al., Material Chemistry and Physics 97 (1) (2006) publishes an article on P151-155), has successfully prepared strontium-barium titanate (BST)/glassy phase complex phase thick-film material.But because the adding of glassy phase reduces the specific inductivity of strontium-barium titanate (BST) pottery greatly, some needs the occasion of high-K capacitor in preparation, and this type of material will be no longer suitable.Thereby, very be necessary to study the specific inductivity that improves this type of material, preparation high-k strontium-barium titanate (BST)/glassy phase material, in order to the range of application of expanding this type of material and develop its potential application may.
Seepage theory provides a kind of thinking for the preparation high-k dielectric materials.Usually, in order to obtain high-k, people often adopt the barium titanate based ceramic material, and add Nb, Ta, and Mn, metal oxides such as Mg are properties-correcting agent.Yet the raising to specific inductivity still is not clearly, and technology is comparatively complicated.Seepage theory is then pointed out, in dielectric, add conductor, continuous increase along with the conductor content that is added, compound system turns to conductor from isolator gradually, and this isolator-conductor transformation is a kind of mutation process, the trace that is the volume fraction of conductor increases, and just can make the specific conductivity of compound system that the variation of some orders of magnitude takes place.Usually, the volume fraction of the conductive phase that contained in the system when realizing that isolator-conductor changes of people calls the seepage flow threshold value.When the volume content of conductor was near the seepage flow threshold value, non-linear enhancing also can take place in the specific inductivity of material.Specific inductivity with the variation of conductor volume content can be with the seepage flow formulate: ε=ε
0| f
c-f|
-q, in the formula, f
cBe the seepage flow threshold value of conductor, f is the volume fraction of conductor, ε
0Be the specific inductivity of insulating body, ε is the specific inductivity of compound system, and q then is a critical exponent of seepage flow system.From this formula as seen, as the volume fraction f＜f of conductor
cAnd f → f
cThe time, conductor-isolator compound system just can obtain the specific inductivity than high times of dielectric substrate.
Therefore, under seepage theory instructs, if consider in strontium-barium titanate (BST)/glassy phase material, to add a certain amount of metallics, make it successfully realize seep effect, in order to improve the specific inductivity of material, then be expected to invent a kind of type material and make it both reduce sintering temperature, improve specific inductivity again greatly, for preparation high-K capacitor under lower temperature has been opened up new direction.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology simple, with low cost, and dielectric properties are good, have the excellent frequency stability and the seepage flow type silver/strontium-barium titanate/nonex matrix material and the preparation method of temperature stability when having ultra-high dielectric coefficient.
Seepage flow type silver/strontium-barium titanate of the present invention/nonex matrix material is with Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Be matrix, mix the matrix material of Ag in matrix, expression formula is Ag/Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3, Ba wherein
0.8Sr
0.2TiO
3/ PbO-B
2O
3Volumn concentration be 99%～70%; The volumn concentration of Ag is 1%～30%.
The preparation method of seepage flow type silver/strontium-barium titanate/nonex matrix material is characterized in that step is as follows:
1) with Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Stoichiometric ratio, take by weighing strontium-barium titanate powder and nonex powder, with strontium-barium titanate powder and nonex powder thorough mixing, obtain matrix powder;
2) ratio of saying in claim 1 takes by weighing matrix powder and silver powder, grinds behind the thorough mixing 1～5 hour, then with the compression moulding of 2～10MPa pressure;
3) with material sintering in air of compression moulding, sintering temperature is 800～900 ℃, and temperature rise rate is controlled at 100～600 ℃/h, and insulation 1～3h obtains seepage flow type silver/strontium-barium titanate/nonex matrix material.
The present invention compares the useful effect that has with background technology: matrix material provided by the present invention is a kind of novel composite material system, prescription is simple, argent is added strontium-barium titanate (BST)/glassy phase material, successfully realized seep effect, reduced the sintering temperature of strontium-barium titanate (BST), the Ag/Ba for preparing
0.8Sr
0.2TiO
3/ PbO-B
2O
3Material and Ba
0.8Sr
0.2TiO system and Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3System material is compared has ultra-high dielectric coefficient (specific inductivity is 24000 during 10KHz).Glassy phase PbO-B in the matrix material that employing the inventive method makes
2O
3Wrap up Ag and BST respectively, Ag and BST are effectively isolated, the matrix material specific inductivity has frequency stability and temperature stability preferably, and has less dielectric loss (dielectric loss is 0.035 during 10KHz), thereby has a good application prospect.
Description of drawings
Fig. 1 is the SEM photo of matrix material of the present invention; (a) Yin percent by volume is 18%, and (b) Yin percent by volume is 22%, and (c) Yin percent by volume is 24%;
Fig. 2 is the curve of the specific inductivity of matrix material of the present invention with frequency change;
Fig. 3 is the curve that the dielectric constant with temperature of matrix material of the present invention changes.
Embodiment
Embodiment 1
With Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Stoichiometric ratio, take by weighing strontium-barium titanate powder and nonex powder, with strontium-barium titanate powder and nonex powder thorough mixing, obtain matrix powder; Press Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Volumn concentration be 99%～70%, the volumn concentration of Ag is 1%～30%, takes by weighing matrix powder and silver powder, grinds behind the thorough mixing 3 hours, then with the compression moulding of 2MPa pressure; With material sintering in air of compression moulding, sintering temperature is 850 ℃, and temperature rise rate is controlled at 600 ℃/h, and insulation 2.5h obtains seepage flow type silver/strontium-barium titanate/nonex matrix material.
The temperature spectrum of relative permittivity, dielectric loss and the specific inductivity of material is tested and calculated to seepage flow type silver/strontium-barium titanate behind the sintering/nonex matrix material 200 ℃ of following burning infiltration silver electrodes, then after surface finish.Test result sees Table 1.Table 1 provides under the 1KHz specific inductivity and dielectric loss with the variation relation (under the room temperature) of metal A g volume content.From table 1, when Ag volume fraction f was between 0.15～0.25, material obtained bigger specific inductivity, and when f=0.23, specific inductivity is 20000, is about 10 times with the body material for preparing under the condition.The specific inductivity of this material has good temperature stability: when temperature was between 0～130 ℃, the change in dielectric constant rate was between 7%～10%.
Fig. 1 is the SEM photo of the matrix material that makes of this example; (a) Yin percent by volume is 18%, and (b) Yin percent by volume is 22%, and (c) Yin percent by volume is 24%;
Table 1
| Ag volume fraction f | 0.01 | 0.15 | 0.2 | 0.22 | 0.23 | 0.25 | 0.26 | 0.30 |
| Specific inductivity | 1571 | 2346 | 5212 | 15980 | 20000 | 15000 | 14300 | 8300 |
| Dielectric loss | 0.067 | 0.081 | 0.093 | 0.17 | 0.3 | 0.43 | 1.5 | 21 |
Embodiment 2
With Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Stoichiometric ratio, take by weighing strontium-barium titanate powder and nonex powder, with strontium-barium titanate powder and nonex powder thorough mixing, obtain matrix powder; Press Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Volumn concentration be 99%～70%, the volumn concentration of Ag is 1%～30%, takes by weighing matrix powder and silver powder, grinds behind the thorough mixing 5 hours, then with the compression moulding of 5MPa pressure; With material sintering in air of compression moulding, sintering temperature is 800 ℃, and temperature rise rate is controlled at 250 ℃/h, and insulation 3h obtains seepage flow type silver/strontium-barium titanate/nonex matrix material.
The temperature spectrum of relative permittivity, dielectric loss and the specific inductivity of material is tested and calculated to seepage flow type silver/strontium-barium titanate behind the sintering/nonex matrix material 200 ℃ of following burning infiltration silver electrodes, then after surface finish.Test result sees Table 2.Table 2 provides under the 1KHz specific inductivity and dielectric loss with the variation relation (under the room temperature) of metal A g volume content.From table 2, when Ag volume fraction f was between 0.18～0.25, material obtained bigger specific inductivity, and when f=0.22, specific inductivity is 24000, is about 12 times with the body material for preparing under the condition.The specific inductivity of this material has good temperature stability: when temperature was between 0～130 ℃, the change in dielectric constant rate was between 8%～10%
Table 2
| Ag volume fraction f | 0.01 | 0.18 | 0.2 | 0.22 | 0.23 | 0.25 | 0.26 | 0.30 |
| Specific inductivity | 1681 | 2456 | 5872 | 24000 | 21000 | 14000 | 13300 | 6300 |
| Dielectric loss | 0.021 | 0.023 | 0.027 | 0.035 | 0.069 | 0.43 | 1.5 | 21 |
Embodiment 3
With Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Stoichiometric ratio, take by weighing strontium-barium titanate powder and nonex powder, with strontium-barium titanate powder and nonex powder thorough mixing, obtain matrix powder; Press Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Volumn concentration be 99%～70%, the volumn concentration of Ag is 1%～30%, takes by weighing matrix powder and silver powder, grinds behind the thorough mixing 1 hour, then with the compression moulding of 10MPa pressure; With material sintering in air of compression moulding, sintering temperature is 900 ℃, and temperature rise rate is controlled at 100 ℃/h, and insulation 1h obtains seepage flow type silver/strontium-barium titanate/nonex matrix material.
The temperature spectrum of relative permittivity, dielectric loss and the specific inductivity of material is tested and calculated to seepage flow type silver/strontium-barium titanate behind the sintering/nonex matrix material 200 ℃ of following burning infiltration silver electrodes, then after surface finish.Test result sees Table 3.Table 3 provides under the 1KHz specific inductivity and dielectric loss with the variation relation (under the room temperature) of metal A g volume content.From table 3, when Ag volume fraction f was between 0.18～0.23, material obtained bigger specific inductivity, and when f=0.23, specific inductivity is 22000, is about 11 times with the body material for preparing under the condition.The specific inductivity of this material has good temperature stability (see figure 3), and when temperature was between 0～130 ℃, the change in dielectric constant rate was between 8%～12%.
The specific inductivity of matrix material of the present invention has frequency stability, sees Fig. 2.
Table 3
| Ag volume fraction f | 0.01 | 0.18 | 0.2 | 0.22 | 0.23 | 0.25 | 0.26 | 0.30 |
| Specific inductivity | 1681 | 2896 | 6892 | 15980 | 20000 | 16000 | 13400 | 5200 |
| Dielectric loss | 0.067 | 0.087 | 0.097 | 0.19 | 0.36 | 0.47 | 1.7 | 25 |
Claims (2)
1. seepage flow type silver/strontium-barium titanate/nonex matrix material is characterized in that it is with Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Be matrix, mix the matrix material of Ag in matrix, expression formula is Ag/Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3, Ba wherein
0.8Sr
0.2TiO
3/ PbO-B
2O
3Volumn concentration be 99%～70%; The volumn concentration of Ag is 1%～30%.
2. the preparation method of the described seepage flow type silver/strontium-barium titanate of claim 1/nonex matrix material is characterized in that step is as follows:
1) with Ba
0.8Sr
0.2TiO
3/ PbO-B
2O
3Stoichiometric ratio, take by weighing strontium-barium titanate powder and nonex powder, with strontium-barium titanate powder and nonex powder thorough mixing, obtain matrix powder;
2) ratio of saying in claim 1 takes by weighing matrix powder and silver powder, grinds behind the thorough mixing 1～5 hour, then with the compression moulding of 2～10MPa pressure;
3) with material sintering in air of compression moulding, sintering temperature is 800～900 ℃, and temperature rise rate is controlled at 100～600 ℃/h, and insulation 1～3h obtains seepage flow type silver/strontium-barium titanate/nonex matrix material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100537074A CN100372803C (en) | 2006-10-08 | 2006-10-08 | Seepage flow type silver/strontium barium titanate/nonex composite material and manufacture method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100537074A CN100372803C (en) | 2006-10-08 | 2006-10-08 | Seepage flow type silver/strontium barium titanate/nonex composite material and manufacture method |
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| Publication Number | Publication Date |
|---|---|
| CN1927764A true CN1927764A (en) | 2007-03-14 |
| CN100372803C CN100372803C (en) | 2008-03-05 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102176355A (en) * | 2011-01-22 | 2011-09-07 | 浙江大学 | Nano Ag particle-(Pb0.4Sr0.6)TiO3 solid solution seepage-type composite ceramic film and preparation method thereof |
| CN105294093A (en) * | 2015-11-11 | 2016-02-03 | 浙江大学 | BTO/NZFO multiphase ceramic having PBO glass phase isolation barrier layer and preparation method thereof |
| CN105842139A (en) * | 2016-04-06 | 2016-08-10 | 清华大学 | Method for determining percolation threshold of pressure-sensitive microspheres in nonlinear insulation material |
| JP2022543027A (en) * | 2019-08-01 | 2022-10-07 | ユニバーシティ オブ マサチューセッツ | Printable mixture, method of making the same, and method of using the same |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003176171A (en) * | 2001-10-04 | 2003-06-24 | Ube Electronics Ltd | Dielectric ceramic composition |
| JP2003160376A (en) * | 2001-11-21 | 2003-06-03 | Ube Electronics Ltd | Dielectric ceramic composition and laminated ceramic part using the same |
| CN100341817C (en) * | 2004-11-18 | 2007-10-10 | 中国电子科技集团公司第五十五研究所 | Preparation method of barium strontium titanate film material |
| CN100382350C (en) * | 2005-12-05 | 2008-04-16 | 浙江大学 | Porous composite thick film pyroelectric material and preparative method |
-
2006
- 2006-10-08 CN CNB2006100537074A patent/CN100372803C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102176355A (en) * | 2011-01-22 | 2011-09-07 | 浙江大学 | Nano Ag particle-(Pb0.4Sr0.6)TiO3 solid solution seepage-type composite ceramic film and preparation method thereof |
| CN102176355B (en) * | 2011-01-22 | 2013-05-22 | 浙江大学 | Nano Ag particle-(Pb0.4Sr0.6)TiO3 solid solution seepage-type composite ceramic film and preparation method thereof |
| CN105294093A (en) * | 2015-11-11 | 2016-02-03 | 浙江大学 | BTO/NZFO multiphase ceramic having PBO glass phase isolation barrier layer and preparation method thereof |
| CN105842139A (en) * | 2016-04-06 | 2016-08-10 | 清华大学 | Method for determining percolation threshold of pressure-sensitive microspheres in nonlinear insulation material |
| JP2022543027A (en) * | 2019-08-01 | 2022-10-07 | ユニバーシティ オブ マサチューセッツ | Printable mixture, method of making the same, and method of using the same |
| JP7325784B2 (en) | 2019-08-01 | 2023-08-15 | ユニバーシティ オブ マサチューセッツ | Printable mixture, method of making the same, and method of using the same |
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|---|---|
| CN100372803C (en) | 2008-03-05 |
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