CN101549998A - Ultra-high dielectric coefficient semiconductor capacitor material and its preparation method - Google Patents
Ultra-high dielectric coefficient semiconductor capacitor material and its preparation method Download PDFInfo
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- CN101549998A CN101549998A CNA2009101140569A CN200910114056A CN101549998A CN 101549998 A CN101549998 A CN 101549998A CN A2009101140569 A CNA2009101140569 A CN A2009101140569A CN 200910114056 A CN200910114056 A CN 200910114056A CN 101549998 A CN101549998 A CN 101549998A
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Abstract
The component and content of the ultra-high dielectric coefficient semiconductor capacitor material is that the mol ratio of SrO-TiO[2]-Nb [2] O [5] is 1:1:0.5 %; the mol ratio of SrO-TiO [2]-La [2] O [3] is 1:1:0.7%; the mol ratio of SrO-TiO [2]-Nb [2] O [5 ]-La [2] O [3] is 1:1:0.7%: 0.4%; 0.3-0.9% mol ratio of CeO [2] is added respectively in each of the above composition. The sample is prepared by performing electronic ceramics conventional process procedure to the component of the material according to the proportioning, after plastic-removing, the sample is placed in a vacuum graphitic carbon pipe furnace for sintering at 1300 DEG C to 1450 DEG C, and furnace cooling after 1.5-2.5 hours, to obtain the semiconductor capacitor material with ultra-high dielectric coefficient. The semiconductor capacitor material has an ultra-high dielectric constant of 1*10<11>, the preparation method is simple, and the invention has safe and reliable performance.
Description
One, technical field
The present invention relates to semiconductor capacitor material preparing technical field, particularly a kind of ultra-high dielectric coefficient semiconductor capacitor material and preparation method thereof.
Two, technical background
Along with equipment such as personal computer, mobile communication are light, thin, short, little day by day, high-performance, in the process of multifunction, more urgent to the requirement of small volume, large-capacity semiconductor electrical condenser.It is little that ultra-high dielectric coefficient N-type semiconductorN electric capacity has a volume, and the characteristics that electrical capacity is big are applicable in the circuit such as loss factor, the less demanding filtering of insulation resistance, bypass, coupling.Document " specific inductivity up to 200,000 semiconductor ceramic capacitor " (" electronic component and material ", 1982, No.4) once report to prepare specific inductivity be 2 * 10
5Semiconductor capacitor material.Chinese patent application CN02125720.5 discloses a kind of ultra-high dielectric coefficient, temperature-stable multilayer ceramic capacitor material and preparation method thereof, and the room temperature dielectric constant of the material of preparation is 4 * 10
3～4.2 * 10
4As seen, present SrTiO
3The specific inductivity of base semiconductor capacitor material is generally less than 10
6, this material can not be satisfied with the microminiaturization and the high performance index request of current electronic component.
SrTiO
3The base semiconductor capacitor material is feeding H mostly
2Perhaps N
2The reduction sintering forms, and causes some problems such as production cost height, complex manufacturing and poor stability to industrial production.Chinese patent application 02134851 discloses has done improvement to sintering schedule, adopts purity nitrogen and liquefied ammonia to decomposite nitrogen, hydrogen gas mixture as the reduction sintering atmosphere, and the supply of the nitrogen of settling a dispute by the parties concerned themselves, hydrogen reduces production cost.Hydrogen content can be controlled in 30%, reduce the higher danger of bringing of density of hydrogen in the high temperature kiln.But, fundamentally do not solve the danger that hydrogen at high temperature explodes and brought easily owing to still adopt hydrogen as reducing atmosphere.
Three, summary of the invention
The purpose of this invention is to provide a kind of ultra-high dielectric coefficient semiconductor capacitor material and preparation method thereof.This preparation method can prepare a kind of ultra-high dielectric coefficient, the semiconductor capacitor material of better performances, and technology is simple, and safety performance is reliable.
The present invention achieves the above object by the following technical programs: a kind of ultra-high dielectric coefficient semiconductor capacitor material and preparation method thereof is provided, and the component of described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.3～0.9%CeO by the mol ratio respectively
2
The component of another described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.3%CeO by the mol ratio respectively
2
The component of another described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.5%CeO by the mol ratio respectively
2
The component of another described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.7%CeO by the mol ratio respectively
2
The component of another described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.9%CeO by the mol ratio respectively
2
The method for preparing described ultra-high dielectric coefficient semiconductor capacitor material, comprise batch mixing, ball milling, drying, granulation, add tackiness agent pre-molding under certain pressure, grind, granulation again, compression moulding gained sample is placed in the muffle furnace at 1～2 hour plastic removal of 750～800 ℃ of insulations, it is characterized in that, be placed on behind the described sample plastic removal in the vacuum graphite carbon pipe furnace in 1300～1450 ℃ of following sintering, be incubated furnace cooling after 1.5～2.5 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material.
The raw material for preparing described ultra-high dielectric coefficient semiconductor capacitor material all adopts analytical reagent.
The concrete grammar and the treatment condition that prepare described ultra-high dielectric coefficient semiconductor capacitor material are as follows:
(1) presses SrO-TiO
2-Nb
2O
5-CeO
2SrO-TiO
2-La
2O
3-CeO
2SrO-TiO
2-Nb
2O
5-La
2O
3-CeO
2Make up described mixed, ball milling is 2～4 hours in ball mill, obtains a kind of batch mixing;
(2) the batch mixing behind the ball milling in loft drier dry 6～8 hours, cross 120 purpose sieve granulations earlier, add tackiness agent pre-molding under 2～5MPa pressure, in the agate alms bowl, ground then 80 mesh sieve once more granulation be pressed into the sample of 1～2mm;
(3) described sample is placed in the muffle furnace at 1～2 hour plastic removal of 750～800 ℃ of insulations, is placed in the vacuum graphite carbon pipe furnace sintering in 1300～1450 ℃ behind the plastic removal, be incubated furnace cooling after 1.5～2.5 hours.
Sample behind sintering room temperature electrical capacity and the resistance of 2693C type LCR digital electric bridge test under 1000Hz, and calculate specific inductivity and resistivity.
The present invention has the following advantages:
1, the semiconductor capacitor material that adopts the method for the invention to be prepared into has 1 * 10
11Ultra-high dielectric coefficient, and the preparation method is simple, is convenient to operation.
2, utilize the vacuum sintering of graphite carbon pipe furnace, improved safety coefficient.
Four, description of drawings
Fig. 1 is preparation method's schema of ultra-high dielectric coefficient semiconductor capacitor material of the present invention.
Fig. 2 is the CeO that undopes
2SrO-TiO
2-Nb
2O
5The XRD spectral line of semiconductor capacitor material.
Fig. 3 is the CeO that undopes
2SrO-TiO
2-La
2O
3The XRD spectral line of semiconductor capacitor material.
Fig. 4 is the CeO that undopes
2SrO-TiO
2-Nb
2O
5-La
2O
3The XRD spectral line of semiconductor capacitor material.
Fig. 5 is the XRD spectral line of the ultra-high dielectric coefficient semiconductor capacitor material of embodiment 1.
Fig. 6 is the XRD spectral line of the ultra-high dielectric coefficient semiconductor capacitor material of embodiment 2.
Fig. 7 is the XRD spectral line of the ultra-high dielectric coefficient semiconductor capacitor material of embodiment 3.
Fig. 8 is the XRD spectral line of the ultra-high dielectric coefficient semiconductor capacitor material of embodiment 4.
Fig. 9 is the XRD spectral line of the ultra-high dielectric coefficient semiconductor capacitor material of embodiment 5.
Five, embodiment
Embodiment 1
Raw material is formed: SrO+TiO
2+ 0.5%Nb
2O
5+ 0.3%CeO
2
According to mol ratio is SrO: TiO
2: Nb
2O
5: CeO
2=1: 1: 0.5%: 0.3% ratio takes by weighing reagent, batch mixing, behind ball milling, drying, granulation, compressing tablet, plastic removal at vacuum graphite carbon pipe furnace in 1300 ℃ of sintered samples, be incubated furnace cooling after 1.5 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material, the performance perameter that test obtains is: electrical capacity C is 0.54F, and DIELECTRIC CONSTANT is 2.56 * 10
11, dielectric loss tangent angle tan α is 0.18, the electricalresistivity is 308.25m.The XRD spectral line of prepared material as shown in Figure 5.
Raw material is formed: SrO+TiO
2+ 0.7%La
2O
3+ 0.7%CeO
2
According to mol ratio is SrO: TiO
2: La
2O
3: CeO
2=1: 1: 0.7%: 0.7% ratio takes by weighing reagent, batch mixing, behind ball milling, drying, granulation, compressing tablet, plastic removal at vacuum graphite carbon pipe furnace in 1300 ℃ of sintered samples, be incubated furnace cooling after 2 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material, the performance perameter that test obtains is: electrical capacity C is 0.54F, and DIELECTRIC CONSTANT is 3.89 * 10
11, dielectric loss tangent angle tan α is 0.06, the electricalresistivity is 30.80 Ω m.The XRD spectral line of prepared material as shown in Figure 6.
Embodiment 3
Raw material is formed: SrO+TiO
2+ 0.7%Nb
2O
5+ 0.4%La
2O
3+ 0.3%CeO
2
According to mol ratio is SrO: TiO
2: Nb
2O
5: La
2O
3: CeO
2=1: 1: 0.7%: 0.4%: 0.3% ratio takes by weighing reagent, batch mixing, behind ball milling, drying, granulation, compressing tablet, plastic removal at vacuum graphite carbon pipe furnace in 1375 ℃ of sintered samples, be incubated furnace cooling after 2.5 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material, the performance perameter that test obtains is: electrical capacity C is 0.54F, and DIELECTRIC CONSTANT is 4.38 * 10
11, dielectric loss tangent angle tan α is 0.05, the electricalresistivity is 1567.35 Ω m.The XRD spectral line of prepared material as shown in Figure 7.
Embodiment 4
Raw material is formed: SrO+TiO
2+ 0.7%Nb
2O
5+ 0.4%La
2O
3+ 0.9%CeO
2
According to mol ratio is SrO: TiO
2: Nb
2O
5: La
2O
3: CeO
2=1: 1: 0.7%: 0.4%: 0.9% ratio takes by weighing reagent, batch mixing, behind ball milling, drying, granulation, compressing tablet, plastic removal at vacuum graphite carbon pipe furnace in 1375 ℃ of sintered samples, be incubated furnace cooling after 2 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material, the performance perameter that test obtains is: electrical capacity C is 0.54F, and DIELECTRIC CONSTANT is 3.33 * 10
11, dielectric loss tangent angle tan α is 1.27, the electricalresistivity is 20.68 Ω m.The XRD spectral line of prepared material as shown in Figure 8.
Embodiment 5
Raw material is formed: SrO+TiO
2+ 0.7%La
2O
3+ 0.5%CeO
2
According to mol ratio is SrO: TiO
2: La
2O
3: CeO
2=1: 1: 0.7%: 0.5% ratio takes by weighing reagent, batch mixing, behind ball milling, drying, granulation, compressing tablet, plastic removal at vacuum graphite carbon pipe furnace in 1450 ℃ of sintered samples, be incubated furnace cooling after 2.5 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material, the performance perameter that test obtains is: electrical capacity C is 0.79F, and DIELECTRIC CONSTANT is 7.31 * 10
11, dielectric loss tangent angle tan α is 0.98, the electricalresistivity is 6.14 Ω m.The XRD spectral line of prepared material as shown in Figure 9.
Utilize the XRD spectral line of jade5.0 software analysis comparison diagram 2 to Fig. 9, the different mol ratio of mixing as can be seen CeO
2Sintered sample have only SrTiO
3Phase, and the XRD spectral line is the same, and adulterated CeO is described
2Be solid-solubilized in SrTiO fully
3In the sill, improved the performance of material.
Claims (6)
1, a kind of ultra-high dielectric coefficient semiconductor capacitor material is characterized in that, the component of described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.3～0.9%CeO by the mol ratio respectively
2
2, ultra-high dielectric coefficient semiconductor capacitor material according to claim 1 is characterized in that, the component of described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.3%CeO by the mol ratio respectively
2
3, ultra-high dielectric coefficient semiconductor capacitor material according to claim 1 is characterized in that, the component of described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.5%CeO by the mol ratio respectively
2
4, ultra-high dielectric coefficient semiconductor capacitor material according to claim 1 is characterized in that, the component of described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.7%CeO by the mol ratio respectively
2
5, ultra-high dielectric coefficient semiconductor capacitor material according to claim 1 is characterized in that, the component of described material and content are:
SrO-TiO
2-Nb
2O
5By the mol ratio is 1: 1: 0.5%
SrO-TiO
2-La
2O
3By the mol ratio is 1: 1: 0.7%
SrO-TiO
2-Nb
2O
5-La
2O
3By the mol ratio is 1: 1: 0.7%: 0.4%
In above-mentioned each composition, mix 0.9%CeO by the mol ratio respectively
2
6, the method for preparing the described ultra-high dielectric coefficient semiconductor capacitor material of claim 1, comprise batch mixing, ball milling, dry, granulation, add tackiness agent pre-molding under certain pressure, grind, granulation again, compression moulding gained sample is placed in the muffle furnace and is incubated 1～2 hour plastic removal at 750～800 ℃, it is characterized in that, is placed on behind the described sample plastic removal in the vacuum graphite carbon pipe furnace in 1300 ℃～1450 ℃ following sintering, be incubated furnace cooling after 1.5～2.5 hours, promptly get described ultra-high dielectric coefficient semiconductor capacitor material.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111103482A (en) * | 2019-12-16 | 2020-05-05 | 肇庆绿宝石电子科技股份有限公司 | Full-automatic test method and system for super capacitor |
| CN113511893A (en) * | 2021-03-24 | 2021-10-19 | 广西大学 | BNT-based high-energy-density ceramic with three-layer structure and preparation method thereof |
-
2009
- 2009-05-12 CN CNA2009101140569A patent/CN101549998A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111103482A (en) * | 2019-12-16 | 2020-05-05 | 肇庆绿宝石电子科技股份有限公司 | Full-automatic test method and system for super capacitor |
| CN113511893A (en) * | 2021-03-24 | 2021-10-19 | 广西大学 | BNT-based high-energy-density ceramic with three-layer structure and preparation method thereof |
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Application publication date: 20091007 |