CN101224984A - Low temperature synthesis of ultra-fine ZnO-SiO2 microwave dielectric ceramic powder by sol-gel method - Google Patents
Low temperature synthesis of ultra-fine ZnO-SiO2 microwave dielectric ceramic powder by sol-gel method Download PDFInfo
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- CN101224984A CN101224984A CNA2008100596315A CN200810059631A CN101224984A CN 101224984 A CN101224984 A CN 101224984A CN A2008100596315 A CNA2008100596315 A CN A2008100596315A CN 200810059631 A CN200810059631 A CN 200810059631A CN 101224984 A CN101224984 A CN 101224984A
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- 239000000843 powder Substances 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 title claims abstract description 25
- 238000003980 solgel method Methods 0.000 title claims description 8
- 229910007676 ZnO—SiO2 Inorganic materials 0.000 title abstract 3
- 230000015572 biosynthetic process Effects 0.000 title description 2
- 238000003786 synthesis reaction Methods 0.000 title description 2
- 239000011701 zinc Substances 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 150000003751 zinc Chemical class 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- LMDAGMAWWYVRJZ-UHFFFAOYSA-N ethanol;zinc Chemical compound [Zn].CCO LMDAGMAWWYVRJZ-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 7
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 150000001298 alcohols Chemical class 0.000 description 9
- 229910004283 SiO 4 Inorganic materials 0.000 description 7
- 239000011858 nanopowder Substances 0.000 description 7
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000003921 particle size analysis Methods 0.000 description 3
- 238000003836 solid-state method Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- DTWCOCYXNRTSIA-UHFFFAOYSA-N C(C)O.[N+](=O)([O-])[O-].[Zn+2].[N+](=O)([O-])[O-] Chemical compound C(C)O.[N+](=O)([O-])[O-].[Zn+2].[N+](=O)([O-])[O-] DTWCOCYXNRTSIA-UHFFFAOYSA-N 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910052844 willemite Inorganic materials 0.000 description 2
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- XKKVXDJVQGBBFQ-UHFFFAOYSA-L zinc ethanol diacetate Chemical compound C(C)O.C(C)(=O)[O-].[Zn+2].C(C)(=O)[O-] XKKVXDJVQGBBFQ-UHFFFAOYSA-L 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
The invention discloses a preparation method of sol-gel to synthesize the ultrafine microwave dielectric ceramic powder of ZnO-SiO2 in the low temperature, which comprises the steps that: the zinc salt and the tetraethyl orthosilicate are respectively dissolved in the anhydrous ethanol to form the ethanol solution of zinc salt and the ethanol solution of tetraethyl orthosilicate; the two solutions are stirred and mixed with the mole ratio of Zn to Si being 2 : 1, then proper anhydrous ethanol is added to control the density of the zinc salt in the mixed solution within a range of 0.5 to 1 mol/l; deionized water is added to promote hydrolytic polymerization; at least one of nitric acid and acrylic acid is added dropwise to adjust the pH value; proper dispersing agent is added to overcome the powder agglomeration; and the gel is obtained after even stirring, sealing and standing of the obtained solution, and then the obtained gel is dried and calcined to obtain the ultrafine microwave dielectric ceramic powder of ZnO-SiO2. The preparation method has the advantages that the ultrafine powder with an adjustable particle size of 80 to 200 nm can be calcined and synthesized under the low temperature condition of 800 to 850 DEG C; and the powder has good microwave property after sintering.
Description
Technical field
The present invention relates to ultra-fine ZnO-SiO
2The preparation method of microwave dielectric ceramic powder especially relates to sol-gel method low temperature synthesizing superfine ZnO-SiO
2The method of microwave dielectric ceramic powder belongs to materials science field.
Background technology
Along with the high speed development of information technology, high frequencyization and the microminiaturized essential characteristic that has become present advanced electronic devices and components.Along with further dwindling of ceramic components volume, the medium layer in the chip multilayer device architecture is also more and more thinner, and an important channel of therefore following preparation ultra-thin medium layer is adopted superfine powder even nanometer grade powder exactly.
Guo.Y etc. are at " J.Eur.Ceram.Soc ", and 2006,26:16-18 " Characterization anddielectric behavior of willemite and TiO
2-doped willemite ceramics atmillimeter-wave frequency " literary composition discloses ZnO-SiO first
2The isostatic cool pressing preparation method of microwave-medium ceramics and microwave property are because its excellent microwave performance causes the concern of vast researcher.Subsequently, " J.Am.Ceram.Soc ", 2007, people such as 90:3127-3130.Nguyen N.H are at " Effect of Zn/Si ratio on the microstructural and microwave dielectrics pro-perties of Zn
2SiO
4Ceramics " literary grace prepares Zn with solid phase method and non-stoichiometric
2SiO
4Pottery and microwave property, non-stoichiometric can be eliminated excessive ZnO to Zn
2SiO
4The ceramic microwave Effect on Performance has obviously been improved quality factor q * f.But up to now, Shang Weijian has employing wet chemical method (containing sol-gel method) to prepare ultra-fine Zn
2SiO
4Pottery is to satisfy the report of ceramic component miniaturization.Sol-gel method is a kind of wet chemical method of comparatively extensive and sophisticated preparation superfine powder of application, can access big, the active big high pure and ultra-fine powder of specific surface area, has been widely used in the preparation of all kinds of electronic ceramics powders.
Summary of the invention
The invention provides a kind ofly, utilize sol-gel method to prepare ultra-fine ZnO-SiO from the requirement of microwave device miniaturization to microwave dielectric ceramic materials powder super-refinement
2The method of microwave dielectric ceramic powder, by the sterically hindered effect of gelation process and dispersion agent, and the process heating and calcining decomposes organism and zinc salt ion generation oxidizing reaction forms crystalline phase, thereby obtains ultra-fine ZnO-SiO at a lower temperature
2Microwave dielectric ceramic powder.
Sol-gel method low temperature synthesizing superfine ZnO-SiO
2The preparation method of microwave dielectric ceramic powder may further comprise the steps:
(1) zinc salt is dissolved in the dehydrated alcohol, forms the zinc salt ethanol solution;
(2) tetraethoxy is dissolved in the ethanol solution, forms the tetraethoxy ethanolic soln;
(3) with zinc salt ethanol solution and tetraethoxy ethanolic soln in zinc: the mol ratio of silicon is that 2: 1 ratio mixes, and adds an amount of dehydrated alcohol, makes that the concentration of zinc salt is controlled at 0.5~1mol/l in the mixing solutions; Add deionized water again, promote hydrolytic process, deionized water: the mol ratio of tetraethoxy transfers to 0~8; Add at least a in nitric acid or the vinylformic acid mixing solutions pH value is transferred to 1~3; Weight in mixing solutions is 100%, adds 1~10% dispersion agent polyoxyethylene glycol PEG;
(4) the above-mentioned mixing solutions that makes is stirred, sealing places 10~40 ℃ of environment, obtains even water white gel; Gel oven dry under 80~100 ℃ is become crisp xerogel;
(5) above-mentioned crisp xerogel is ground, put into the high alumina crucible,, obtain the ZnO-SiO of white 600~1000 ℃ of calcinings
2Microwave dielectric ceramic powder.
Described zinc salt is Zn (NO
3)
26H
2O, Zn (CH
3COOH)
22H
2O, ZnCl
2
Adopt above-mentioned technology, can obtain particle diameter at 100~200nm and finely disseminated ultra-fine ZnO-SiO
2Microwave dielectric ceramic powder, this superfine powder have higher Q * f value after sintering porcelain into, compare, are significantly improved with the Q * f value after the synthetic micro-powder of conventional solid-state method sinters porcelain into; And its sintering temperature has descended 100~150 ℃ with respect to the sintering temperature of solid phase method gained micro-powder.Can be used for preparing ultra-thin cast film and miniature chip multiplayer microwave device, have great industrial application value.Preparation method of the present invention has following characteristics:
(1) adopts Zn (NO
3)
26H
2O, Zn (CH
3COOH)
22H
2O, ZnCl
2Deng zinc salt is raw material, and low price and raw material are easy to get;
(2) adopt wet chemical method that zinc, element silicon are evenly distributed in the colloidal sol, utilize the sterically hindered effect of gelation process and dispersion agent, the Chemical Composition that makes final product evenly and also the diameter of particle that obtains after the calcining tiny;
(3) can after 800 ℃ of calcinings, obtain ultra-fine ZnO-SiO
2Microwave dielectric ceramic powder greatly reduces ZnO-SiO
2The synthesis temperature of powder, the superfine powder particle diameter that obtains is adjustable between 100~200nm, and good dispersion;
(4) the ultra-fine ZnO-SiO of this method synthetic
2Microwave-medium ceramics can sinter porcelain at 1250 ℃, than the synthetic micron ZnO-SiO of conventional solid-state method
2The sintering temperature of powder (1400 ℃) has descended about 150 ℃; This nano-powder has higher Q * f value after sintering porcelain into, and the Q * f value of synthesizing after micro-powder sinters porcelain into than conventional solid-state method improves 20%.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
Take by weighing the Zn (NO of 1mol
3)
2.6H
2O is dissolved in 475 milliliters of dehydrated alcohols, forms the zinc nitrate ethanol solution that concentration is about 2.0mol/l; The tetraethoxy of 0.5mol is mixed with 110 milliliters of dehydrated alcohols, form the tetraethoxy ethanolic soln; Above-mentioned two solution are mixed, stir, add 550 milliliters of dehydrated alcohols, making zinc concentration is 0.8mol/l.Add the 3mol deionized water then, 8 gram concentration are 65~68% concentrated nitric acid, 20 gram PEG400, the pH value of solution is 1.5.
After above-mentioned mixing solutions stirred, be statically placed in 30 ℃ the water-bath, obtain water white gel, gel is taken out put into pallet, 80 ℃ dry 24 hours down, obtain crisp material.
Above-mentioned crisp material is ground, put into the high alumina crucible,, obtain the ZnO-SiO of white 800 ℃ of calcinings 1 hour
2Microwave dielectric ceramic powder.
This material is through TEM Electronic Speculum and laser particle size analysis, and the powder median size is between 100~200nm, and dispersion of particles is good; XRD analysis shows that the principal crystalline phase of this nano-powder is Zn
2SiO
4
With above-mentioned nano-powder grinding, the granulation that obtains 800 ℃ of calcinings, be pressed into the nahlock of diameter 18mm, height 8~9mm, at 1250 ℃ of sintering 30min, its microwave dielectric property is: ε
r=6.14, Qf=67500GHz.
Embodiment 2:
Take by weighing the Zn (CH of 0.5mol
3COOH)
22H
2O is dissolved in 320 milliliters of dehydrated alcohols, forms the zinc acetate ethanol solution that concentration is about 1.5mol/l; The tetraethoxy of 0.25mol is mixed with 115 milliliters of dehydrated alcohols, form the tetraethoxy ethanolic soln; Above-mentioned two solution are mixed, stir, add 400 milliliters of dehydrated alcohols, making zinc concentration is 0.6mol/l.Add 2mol deionized water, 3 gram concentration then and be 65~68% concentrated nitric acid and 4 gram vinylformic acid, 10 gram PEG1000, the pH value of solution is 2.
After above-mentioned mixing solutions stirred, be statically placed in 35 ℃ the water-bath, obtain water white gel, gel is taken out put into pallet, 90 ℃ dry 24 hours down, obtain crisp material.
Above-mentioned crisp material is ground, put into the high alumina crucible,, obtain the ZnO-SiO of white 850 ℃ of calcinings 1 hour
2Microwave dielectric ceramic powder.
This material is through TEM Electronic Speculum and laser particle size analysis, and the powder median size is between 120~180nm, and dispersion of particles is good; XRD analysis shows that the principal crystalline phase of this nano-powder is Zn
2SiO
4
With above-mentioned nano-powder grinding, the granulation that obtains 850 ℃ of calcinings, be pressed into the nahlock of diameter 18mm, height 8~9mm, at 1250 ℃ of sintering 30min, its microwave dielectric property is: ε
r=6.32, Qf=70300GHz.
Embodiment 3:
Take by weighing the Zncl of 0.5mol
2Be dissolved in 115 milliliters of dehydrated alcohols, form the zinc nitrate ethanol solution that concentration is about 4mol/l; The tetraethoxy of 0.25mol is mixed with 110 milliliters of dehydrated alcohols, form the tetraethoxy ethanolic soln; Above-mentioned two solution are mixed, stir, add 250 milliliters of dehydrated alcohols, making zinc concentration is 1.0mol/l.Add the 1mol deionized water then, 2.5 gram concentration are 65~68% concentrated nitric acid, 8 gram PEG1000, the pH value of solution is 2.5.
After above-mentioned mixing solutions stirred, be statically placed in 30 ℃ the water-bath, obtain water white gel, gel is taken out put into pallet, 80 ℃ dry 24 hours down, obtain crisp material.
Above-mentioned crisp material is ground, put into the high alumina crucible,, obtain the ZnO-SiO of white 800 ℃ of calcinings 1 hour
2Microwave dielectric ceramic powder.
This material is through TEM Electronic Speculum and laser particle size analysis, and the powder median size is between 150~280nm, and dispersion of particles is good; XRD analysis shows that the principal crystalline phase of this nano-powder is Zn
2SiO
4
With above-mentioned nano-powder grinding, the granulation that obtains 800 ℃ of calcinings, be pressed into the nahlock of diameter 18mm, height 8~9mm, at 1250 ℃ of sintering 30min, its microwave dielectric property is: ε
r=6.25, Qf=65300GHz.
Claims (2)
1. one kind is utilized sol-gel method low temperature synthesizing superfine ZnO-SiO
2The preparation method of microwave dielectric ceramic powder may further comprise the steps:
(1) zinc salt is dissolved in the dehydrated alcohol, forms the zinc salt ethanol solution;
(2) tetraethoxy is dissolved in the ethanol solution, forms the tetraethoxy ethanolic soln;
(3) with zinc salt ethanol solution and tetraethoxy ethanolic soln by zinc: the mol ratio of silicon is 2: 1 a mixed, adds dehydrated alcohol, makes that the concentration of zinc salt is controlled at 0.5~1mol/l in the mixing solutions; Add deionized water again, promote hydrolytic process, deionized water: the mol ratio of tetraethoxy transfers to 0~8; Add at least a in nitric acid or the vinylformic acid mixing solutions pH value is transferred to 1~3; Weight in mixing solutions is 100%, adds 1~10% dispersion agent polyoxyethylene glycol PEG;
(4) the above-mentioned mixing solutions that makes is stirred, sealing places 10~40 ℃ of environment, obtains even water white gel; Gel oven dry under 80~100 ℃ is become crisp xerogel;
(5) above-mentioned crisp xerogel is ground, put into the high alumina crucible,, obtain the ZnO-SiO of white 600~1000 ℃ of calcinings
2Microwave dielectric ceramic powder.
2. preparation method according to claim 1 is characterized in that: described zinc salt is Zn (NO
3)
26H
2O or Zn (CH
3COOH)
22H
2O or ZnCl
2
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