CN102120703A - High solid content lithium-niobium-titanium series microwave medium ceramic water-based casting green tape - Google Patents
High solid content lithium-niobium-titanium series microwave medium ceramic water-based casting green tape Download PDFInfo
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Abstract
The invention relates to a high solid content lithium-niobium-titanium series microwave medium ceramic water-based casting green tape, belonging to the preparation field of the microwave medium ceramic. In the preparation method of the green tape, lithium-niobium-titanium series low temperature sintered microwave medium ceramic is used as solid phase powder, water is used as solvent, styrene-acrylic emulsion is used as binder, and plasticizer, dispersant, defoaming agent, film-forming additive and the like are added to prepare ceramic slurry, and the casting and drying technology is performed to prepare the green tape. The prepared water-based microwave medium ceramic green tape has high solid content, smooth surface, good mechanical propertics, no pollution and low cost; electrode materials such as silver and copper can be printed on the surface of the green tape, binder is removed at 400-450 DEG C and the product is sintered at 860-950 DEG C to have excellent microwave dielectric properties. The green tape material is suitable to prepare multi-layer low temperature cofired ceramic (LTCC) electronic components such as chip dielectric resonators, filters, Baluns and antennas and has broad application prospect.
Description
Technical field
The present invention relates to a kind of high solids content series of lithium, niobium and titanium microwave dielectric ceramic aqueous tape casting and give birth to band, belong to the microwave-medium ceramics preparation field.
Technical background
Li
2O-Nb
2O
5-TiO
2Series microwave dielectric ceramic has the excellent microwave dielectric properties, its specific inductivity is 20～80, quality factor height and temperature coefficient of resonance frequency are low, the living band of this material is applicable to and designs and produces sheet medium resonator, wave filter, Ba Lun, antenna and multilayer LTCC (LTCC) electronic devices and components such as multilayered structure bluetooth, GPS module etc., is with a wide range of applications.Borisevich, Davies and domestic Shanghai Silicate Inst., Chinese Academy of Sciences [patent 1, publication number CN 1915904A], [patent 2, publication number CN 1821171A] and Xi'an Communications University [patent 3, publication number CN 101224977A] etc. it has been carried out big quantity research.Li
2O-Nb
2O
5-TiO
2System is the material system of a kind of intrinsic sintering temperature low (～1100 ℃), and a kind of " M-phase " sosoloid Li is arranged in this system
1+x-yNb
1-x-3yTi
X+4yO
3, this " M-phase " has lower sintering temperature (pure " M-phase " is not higher than 1100 ℃), is a kind of low-temperature sintering microwave medium material of excellent performance, by adding sintering aid its sintering temperature can be reduced to below 960 ℃.
Shanghai Silicate Inst., Chinese Academy of Sciences has mentioned a kind of series of lithium, niobium and titanium low-temperature sintering microwave medium pottery with two-phase composite structure at [patent 1, publication number CN 1915904A], and its material molar ratio is Li
2O: Nb
2O
5: TiO
2=5: x: y, wherein 1≤x＜2; 4＜y＜6, this microwave-medium ceramics is by Li
2TiO
3Sosoloid and M-be the composite structure of sosoloid two phase composites, wherein Li mutually
2TiO
3The Li of sosoloid
2O, Nb
2O
5, TiO
2Mol ratio is 5: 0.583: 3.248, and its specific inductivity is about 20, and the about 13ppm/ of temperature coefficient of resonance frequency ℃, Q * f can reach 50000GHz, has excellent microwave dielectric property.
The green band that uses casting technique to make microwave dielectric ceramic materials has become laminated ceramic capacitor, chip microwave device, the LTCC essential primary material of function ceramics such as (LTCC), has a wide range of applications in Electronic Packaging, circuit substrate, passive component field.Though the green band is a kind of intermediates, but the moulding of electrode component, little packaging technologies such as punching, through hole filling, metallization, circuit printing all are to carry out on the green band, the electronic ceramics quality product depends on the quality of green band to a great extent, therefore develops the key that high performance low-temperature sintering microwave medium green band becomes the exploitation of function ceramics field.
From the solvent species of ceramic green band with slurry, casting technique comprises two kinds of organic and water-based tape castings, from domestic and international research situation in recent years, the casting technique of organic solvent is comparative maturity, it is short that the ceramic green band of preparation has time of drying, even structure, the intensity height, characteristics such as snappiness is good, be widely used in the suitability for industrialized production, but because organic solvent has inflammable, poisonous and the high shortcoming of production cost, with an organic solvent will bring production safety hidden danger and environmental pollution in a large number, harmful to HUMAN HEALTH, therefore, research has become irreversible trend with water as the curtain coating technology of solvent replace organic solvent.The water-based flow casting technique production cost is low, safe in utilization and be convenient to scale operation, environmentally friendly, but technically also there is more difficult point in it, need add with aqueous solution form as binding agent, and the slurry solid content is low; The slurry degasification is difficulty, and the existence of bubble can influence living belt surface smooth finish; The ceramic green sheet snappiness is relatively poor behind the casting film-forming, occurs crack defect easily, and intensity is not high.Can improve water base quality problems of giving birth to band by selecting suitable binding agent and suitable addition.
Binding agent is a most important moiety in the casting slurry, mainly plays to connect the ceramic powder particle in giving birth to band, and living band strength is provided, the effect of control rheological behaviour.The raising of giving birth to the band solid content will improve the density of giving birth to band, finally significantly improve the performance of slice component product; If the content of water in the reduction slurry, then slurry viscosity is too high, and is influential to casting technique.Therefore selection of binder is even more important in the water-based slurry preparation with collocation.Because the used binding agent of water-based slurry mostly is emulsion form, product is less on the market, and selection of binder is restricted.At present, studying water based adhesive more, the technology comparative maturity is polyvinyl alcohol (PVA), and PVA makees binding agent, the ceramic green band strength height of institute's curtain coating, and favourable follow-up little packaging technology, but in the casting slurry layoutprocedure, PVA and sintering aid B commonly used
2O
3A kind of gel reaction can take place, and has increased the viscosity of slurry, thereby has destroyed the original flowability of slurry; And the concentration of aqueous solution of PVA is low, and the content that causes water in the formula of size is too high and can't improve the powder solid content.Zhejiang University is in [patent 4, publication number CN 101328069A] and [patent 5, publication number CN 101328068A] in used PVA and polyacrylic acid (PAA) to prepare the series of lithium, niobium and titanium microwave dielectric ceramic aqueous tape casting to give birth to band as binding agent, lithium niobium titanium ceramic content has brought up to 60% in its slurry.And the latex system is made binding agent, and, ceramic powder solid content height low because of its slurry viscosity, rate of drying are fast, the low advantage such as burn off that is easier to of organic content, becomes the research focus of new water based adhesive gradually.
Summary of the invention
The object of the invention provides a kind of high solids content series of lithium, niobium and titanium microwave dielectric ceramic aqueous tape casting and gives birth to band.The present invention adopts the series of lithium, niobium and titanium low-temperature sintered microwave dielectric ceramic material, can reduce sintering temperature to 860～950 ℃ behind a small amount of sintering aid by adding, by selecting suitable binding agent, softening agent and other functional agents, prepare solid content height, smooth surface, intensity height, be applicable to that the water-based tape casting microwave-medium ceramics of LTCC (LTCC) technology gives birth to band through casting technique.As the solvent in the casting technique, the employing benzene emulsion is a binding agent with water in the present invention, and benzene emulsion is that the form of 47～49% water-based emulsion adds with concentration, and softening agent preferentially adopts glycerol, and the mass ratio of itself and binding agent is between 1: 5～4: 5; Dispersion agent preferentially adopts ammonium polyacrylate, and the per-cent that the dispersion agent add-on accounts for stock quality is 0.5%～2%; Defoamer accounts for the per-cent 0.01%～0.1% of slurry total mass; The per-cent that the add-on of other film coalescence aid accounts for the slurry total mass is 0.05%～1%.Its casting technique is as follows:
1, water and dispersant is even, it is dispersion agent that the present invention selects ammonium polyacrylate for use.With series of lithium, niobium and titanium microwave dielectric ceramic powder and sintering aid V
2O
5Add in the mixed solution and be mixed with slurry;
2, the slurry with step 1 preparation carries out ball milling, and the time is 12～24h;
3, binding agent benzene emulsion and softening agent, defoamer and film coalescence aid are added the slurry that step 2 prepares step by step, continue ball milling 6～12h;
4, the slurry suction filtration that step 3 is prepared, vacuum stirring de-bubble then;
5, the slurry with step 4 preparation carries out curtain coating, behind 30～60 ℃ of drying 1～3h, obtains the ceramic green band;
Material prints electrode on the ceramic green belt surface with preparation, low-temperature sintering moulding then, the sintering program is as follows: be warming up to 400～450 ℃ with the speed of 2～3 ℃/min and carry out binder removal, the binder removal time is controlled at 60～100mins, be warming up to 860～950 ℃ with the speed of 6～8 ℃/min then and carry out sintering, sintering time is controlled at 60～120mins.
The series of lithium, niobium and titanium microwave dielectric ceramic powder that the present invention adopts is preferred a kind of by Li
2TiO
3Sosoloid and M-be the composite ceramic material of sosoloid two phase composites mutually, has the low and excellent microwave dielectric property of intrinsic sintering temperature, is highly suitable for low temperature co-fired (LTCC) multilayer sheet type electronic devices and components.The present invention adds low melting point oxide V in microwave dielectric ceramic powder
2O
5Make sintering aid, utilize its liquid phase sintering mechanism, the ceramic green band can (be lower than electrode materials fusing points such as silver, copper) at low temperatures densified sintering product.The present invention selects for use benzene emulsion to make binding agent, and itself and series of lithium, niobium and titanium microwave dielectric ceramic powder associativity are good, and the adding of benzene emulsion simultaneously can reduce slurry viscosity, avoids destroying because of the adding of sintering aid the flowability of slurry.The concentration of the styrene-acrylate in the benzene emulsion greatly reduces the content of water in the formula of size near 50%, thereby improves solid content, and improves the surface tension and the de-bubble effect of slurry, improves the surface smoothness that curtain coating is given birth to band.
The invention has the advantages that:
(1) adopt water-based flow casting technique, preparation technology is simple, satisfies environmental requirement, and cost is low, is fit to large-scale industrial production.
(2) add low melting point oxide V
2O
5Make sintering aid, give birth to band and can burn altogether with electrode materialss such as silver, copper down, and avoid because of adding B at 860～950 ℃
2O
3The pulp gel problem that may bring and add lead-containing materials and the problem of environmental pollution that brings.
(3) the preferential employing has two-phase (Li
2TiO
3Sosoloid and M-be sosoloid mutually) the series of lithium, niobium and titanium microwave dielectric ceramic materials of composite structure makes to give birth to the band solid phase, its specific inductivity is 34～50, quality factor height and temperature coefficient of resonance frequency are low, is fit to design and produce multilayer LTCC (LTCC) electronic devices and components such as sheet medium resonator, wave filter, Ba Lun, antenna;
(4) selecting benzene emulsion for use is binding agent, has not only improved living band solid content of slurry but also has guaranteed the flowability of slurry, improves the surface smoothness of giving birth to band.
Embodiment
In conjunction with content of the present invention, provide following specific embodiment.
Embodiment 1:
0.8 gram ammonium polyacrylate is joined in the 15 gram water, stir the back and add 62 gram lithium niobium titanium dielectric ceramic powders and 1 gram V
2O
5Powder, it is standby to make water-based slurry behind the ball milling 12h.With 15.8 gram concentration is that 48% benzene emulsion, 5 gram glycerol, 0.08 gram defoamer and 0.32 gram film coalescence aid etc. join in the water-based slurry of getting ready step by step, continues to obtain water base ceramic size behind the ball milling 6h.The gained slurry after filtration, after the vacuum stirring de-bubble on casting machine curtain coating, obtain microwave-medium ceramics behind the dry 3h down at 60 ℃ and give birth to band.Carry out inserting in the sintering oven after the cutting to giving birth to band, be warming up to 450 ℃ with the speed of 2 ℃/min and carry out binder removal, the binder removal time is controlled at 100mins, and the speed with 6 ℃/min is warming up to 880 ℃ of sintering then, obtains the microwave dielectric ceramic diaphragm of compact structure behind the sintering 100mins.
Embodiment 2:
0.9 gram ammonium polyacrylate is joined in the 14 gram water, stir the back and add 65 gram lithium niobium titanium dielectric ceramic powders and 1.3 gram V
2O
5Powder, it is standby to make water-based slurry behind the ball milling 18h.With 14.5 gram concentration is that 48% benzene emulsion, 4 gram glycerol, 0.06 gram defoamer and 0.24 gram film coalescence aid etc. join in the water-based slurry of getting ready step by step, continues to obtain water base ceramic size behind the ball milling 8h.The gained slurry after filtration, after the vacuum stirring de-bubble on casting machine curtain coating, obtain microwave-medium ceramics behind the dry 2.5h down at 50 ℃ and give birth to band.Carry out inserting in the sintering oven after the cutting to giving birth to band, be warming up to 435 ℃ with the speed of 2 ℃/min and carry out binder removal, the binder removal time is controlled at 100mins, and the speed with 6 ℃/min is warming up to 900 ℃ of sintering then, obtains the microwave dielectric ceramic diaphragm of compact structure behind the sintering 100mins.
Embodiment 3:
1 gram ammonium polyacrylate is joined in the 13 gram water, stir back adding 68 grams and have two-phase (M-phase sosoloid and Li
2TiO
3Sosoloid) Li of composite structure
1.429Nb
0.286Ti
0.786O
3(its material molar ratio is Li to dielectric ceramic powder
2O: Nb
2O
5: TiO
2=5: 1: 1.5) and 1.4 the gram V
2O
5Powder, it is standby to make water-based slurry behind the ball milling 20h.With 13.2 gram concentration is that 48% benzene emulsion, 3.2 gram glycerol, 0.04 gram defoamer and 0.16 gram film coalescence aid etc. join in the water-based slurry of getting ready step by step, continues to obtain water base ceramic size behind the ball milling 10h.The gained slurry after filtration, after the vacuum stirring de-bubble on casting machine curtain coating, obtain microwave-medium ceramics behind the dry 2h down at 50 ℃ and give birth to band.Carry out inserting in the sintering oven after the cutting to giving birth to band, be warming up to 435 ℃ with the speed of 2 ℃/min and carry out binder removal, the binder removal time is controlled at 80mins, speed with 7 ℃/min is warming up to 920 ℃ of sintering then, obtain compact structure, quality factor height and the low microwave dielectric ceramic diaphragm of temperature coefficient of resonance frequency behind the sintering 110mins
Embodiment 4:
0.9 gram ammonium polyacrylate is joined in the 11.5 gram water, stir the back and add 72 gram lithium niobium titanium dielectric ceramic powders and 1.6 gram V
2O
5Powder, it is standby to make water-based slurry behind the ball milling 24h.With 11.4 gram concentration is that 48% benzene emulsion, 2.5 gram glycerol, 0.02 gram defoamer and 0.08 gram film coalescence aid etc. join in the water-based slurry of getting ready step by step, continues to obtain water base ceramic size behind the ball milling 12h.The gained slurry after filtration, after the vacuum stirring de-bubble on casting machine curtain coating, obtain microwave-medium ceramics behind the dry 2h down at 40 ℃ and give birth to band.Carry out inserting in the sintering oven after the cutting to giving birth to band, be warming up to 430 ℃ with the speed of 3 ℃/min and carry out binder removal, the binder removal time is controlled at 80mins, and the speed with 8 ℃/min is warming up to 950 ℃ of sintering then, obtains the microwave dielectric ceramic diaphragm of compact structure behind the sintering 120mins.
Claims (8)
1. a high solids content series of lithium, niobium and titanium microwave dielectric ceramic aqueous tape casting is given birth to band, and its casting slurry comprises series of lithium, niobium and titanium microwave dielectric ceramic powder, water solvent, binding agent, softening agent, dispersion agent, defoamer and other film coalescence aid, it is characterized in that:
(1) be the slurry solid phase with the series of lithium, niobium and titanium microwave dielectric ceramic powder, its quality accounts for the per-cent of slurry total mass greater than 61%;
(2) with water as the primary solvent in the casting slurry configuration;
(3) with the benzene emulsion be binding agent;
(4) above-mentioned aqueous medium ceramic green band casting slurry (mass percent) composed as follows:
Water: 11～17%; Lithium niobium titanium valve body: 61～72%;
Sintering aid: 1～2%; Benzene emulsion: 10～20%;
Softening agent: 2～8%; Dispersion agent: 0.5～2%;
Defoamer: 0.01～0.1%; Film coalescence aid: 0.05～0.5%
2. according to the described aqueous medium ceramic green of claim 1 band casting slurry, it is characterized in that described series of lithium, niobium and titanium microwave-medium ceramics is preferably by Li
2TiO
3Sosoloid and M-be the composite structure of sosoloid two phase composites mutually, and the meso-position radius of its powder is not more than 3.0 μ m.
3. according to the described aqueous medium ceramic green of claim 1 band casting slurry, it is characterized in that described sintering aid is low melting point oxide V
2O
5
4. according to the described aqueous medium ceramic green of claim 1 band casting slurry, it is characterized in that described binding agent benzene emulsion is the styrene-acrylate copolymer emulsion, is the water-based emulsion of a kind of solid content between 47～49%.
5. according to the described aqueous medium ceramic green of claim 1 band casting slurry, it is characterized in that the preferred glycerol of described softening agent, its add-on accounts for the per-cent preferred 3～6% of slurry total mass.
6. according to the described aqueous medium ceramic green of claim 1 band casting slurry, the mass ratio that it is characterized in that softening agent glycerol and binding agent is between 1: 5～4: 5, and its preferred mass ratio is between 1: 4～3: 4.
7. according to the described aqueous medium ceramic green of claim 1 band casting slurry, it is characterized in that described dispersion agent optimization polypropylene acid ammonium, its add-on accounts for the per-cent preferred 0.8～1.5% of slurry total mass.
8. according to the described aqueous medium ceramic green of claim 1 band casting slurry, it is characterized in that described defoamer does not preferably contain the mineral oil of VOC.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701730A (en) * | 2012-06-25 | 2012-10-03 | 景德镇陶瓷学院 | Calcium strontium lithium samarium titanium system microwave dielectric ceramic water-base tape-casting slurry and method for preparing ceramic diaphragm |
| CN102976752A (en) * | 2012-12-05 | 2013-03-20 | 景德镇陶瓷学院 | Potassium-sodium niobate base textured piezoelectric ceramics water base tape casting slurry, and preparation method for ceramic membrane therefrom |
| CN103360060A (en) * | 2013-07-19 | 2013-10-23 | 景德镇陶瓷学院 | Sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry and preparation method of ceramic membrane thereof |
| CN105121387A (en) * | 2013-03-15 | 2015-12-02 | 通用电气公司 | Slurries for composite materials |
| CN108314430A (en) * | 2018-03-13 | 2018-07-24 | 中国建筑材料科学研究总院有限公司 | A kind of Cellulose nanocrystal modified ceramic curtain coating green body and preparation method thereof |
| CN116284914A (en) * | 2023-05-22 | 2023-06-23 | 山东森荣新材料股份有限公司 | Preparation method and application of composite dielectric substrate |
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| CN101328069A (en) * | 2008-07-28 | 2008-12-24 | 浙江大学 | Preparation of microwave dielectric ceramic diaphragm by aqueous tape casting forming |
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2010
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701730A (en) * | 2012-06-25 | 2012-10-03 | 景德镇陶瓷学院 | Calcium strontium lithium samarium titanium system microwave dielectric ceramic water-base tape-casting slurry and method for preparing ceramic diaphragm |
| CN102976752A (en) * | 2012-12-05 | 2013-03-20 | 景德镇陶瓷学院 | Potassium-sodium niobate base textured piezoelectric ceramics water base tape casting slurry, and preparation method for ceramic membrane therefrom |
| CN105121387A (en) * | 2013-03-15 | 2015-12-02 | 通用电气公司 | Slurries for composite materials |
| US11319253B2 (en) | 2013-03-15 | 2022-05-03 | General Electric Company | Slurries for composite materials |
| CN103360060A (en) * | 2013-07-19 | 2013-10-23 | 景德镇陶瓷学院 | Sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry and preparation method of ceramic membrane thereof |
| CN103360060B (en) * | 2013-07-19 | 2014-11-19 | 景德镇陶瓷学院 | Sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry and preparation method of ceramic membrane thereof |
| CN108314430A (en) * | 2018-03-13 | 2018-07-24 | 中国建筑材料科学研究总院有限公司 | A kind of Cellulose nanocrystal modified ceramic curtain coating green body and preparation method thereof |
| CN116284914A (en) * | 2023-05-22 | 2023-06-23 | 山东森荣新材料股份有限公司 | Preparation method and application of composite dielectric substrate |
| CN116284914B (en) * | 2023-05-22 | 2023-08-15 | 山东森荣新材料股份有限公司 | Preparation method and application of composite dielectric substrate |
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Application publication date: 20110713 |