CN102030525A - Low-temperature sintered magnesium titanate ceramic and preparation method thereof - Google Patents
Low-temperature sintered magnesium titanate ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses low-temperature sintered magnesium titanate ceramic and a preparation method thereof. The preparation method comprises the following steps of: dissolving compounds containing titanium, magnesium, calcium, zinc, barium and other elements, tetraethoxysilane, boric acid and the like into absolute ethanol to form a mixed solution; controlling the pH value of the system and adding a proper amount of deinized water to obtain transparent gel; drying the gel and then calcining the dried gel at the temperature of 650-850 DEG C to obtain ceramic powder; adding a bonding agent in the powder; and granulating, forming and discharging gel and sintering at the temperature of 890-1,100 DEG C to obtain the low-temperature sintered magnesium titanate ceramic. The method has a simple process; a magnesium titanate matrix is mixed with a singer addictive in the atomistic level by using the sol-gel process; and on the premise of reducing the consumption of the addictive as much as possible, by using the synergism of superfine power grain size and the sintering addictive, the sintering temperature of the ceramic can be effectively lowered and the microwave dielectric property can be obtained.
Description
Technical field
The present invention relates to a kind of low-temperature sintering magnesium titanate ceramics and preparation method thereof, belong to materials science field.
Background technology
Magnesium titanate ceramics has characteristics such as specific inductivity is moderate, dielectric loss is low, frequency-temperature coefficient is little, add its abundant raw material, with low cost, become one of at present most widely used microwave dielectric ceramic materials, and be widely used in the chip multilayer microwave device for preparing moving communicating field, as chip multilayer microwave ceramic capacitance device, gps antenna, sheet medium wave filter and chip resonator etc.For preparing high performance chip multilayer microwave device, magnesium titanate ceramics and metal electrode need be carried out low temperature co-firedly, metal electrode material commonly used at present mainly contains 30Pd-70Ag (1167 ℃ of fusing points), copper (1083 ℃ of fusing points), silver (961 ℃ of fusing points).Yet the sintering temperature of magnesium titanate ceramics is up to 1400 ℃, for realizing low temperature co-fired with above-mentioned electrode materials, must reduce its sintering temperature.
For reducing the sintering temperature of magnesium titanate ceramics, mainly realize at present by following two kinds of approach.A kind of approach is that employing nano level metatitanic acid magnesium powder is a raw material, utilizes the high-ratio surface of nano-powder can promote ceramic dense sintering, reduces its sintering temperature.As Miao etc. (Mater Sci Eng B, 2006,128:103) adopt sol-gel method to synthesize the magnesium titanate powder of 10-30nm, the sintering temperature of magnesium titanate ceramics has been reduced to 1200 ℃ from 1400 ℃, and has obtained good microwave dielectric property: ε
r=16.6, Q * f=42,600, τ
f=-41ppm/ ℃.Yet, limited with nano-powder as the effect that raw material reduces the magnesium titanate ceramics sintering temperature, the sintering temperature of above-mentioned nano barium titanate magnesium powder is difficult to the low temperature co-fired of realization and metal electrode about 1200 ℃, do not possess actual application value in chip multilayer microwave device field.
Another important channel that reduces the magnesium titanate ceramics sintering temperature is to add an amount of low-temperature sintering auxiliary agent.For example Huang etc. (Mater Res Bull, 2001,36:2741) by adding B
2O
3The sintering temperature of pottery is reduced to 1200 ℃; Bernard etc. (J Eur Ceram Soc, 2004,24:1877) at MgTi
0.975O
3In add LiF, the sintering temperature of pottery is reduced to 1000 ℃; Chen etc. (Mater Chem Phys, 2003,79:129) press MgCaTiO
3/ BaBSiO glass is 50/50 proportioning, has obtained the pottery of dense structure at 900 ℃ of sintering, and its dielectric properties are: ε
r=13.2, Q * f=10000; Jantunen etc. (J EurCeram Soc, 2000,20:2331) with the MgTiO of 30wt%
3-CaTiO
3The RO-B of base-material and 70wt%
2O
3-SiO
2(R=Zn, Ba) glass has been realized low-temperature sintering at 900 ℃, the dielectric properties of acquisition are: ε
r=8.5, Q * f=8800 (8GHz).
In the method for above-mentioned reduction magnesium titanate ceramics sintering temperature, it is the simplest, the most effective adding the low-temperature sintering auxiliary agent, also is the cheapest a kind of method of price.But the introducing of a large amount of low-temperature sintering auxiliary agents, to the microwave dielectric property of magnesium titanate ceramics be had a negative impact, particularly in the magnesium titanate powder, add the glass powder and the micron-sized oxides additive of big particle, behind sintering, be distributed in the magnesium titanate grain boundary mutually, worsen the microwave dielectric property of pottery residual a large amount of second.Therefore, as far as possible on the basis of reducing the low-temperature sintering additive dosage, farthest reduce the sintering temperature of magnesium titanate ceramics, not only help saving the shared material cost of sintering aid, also will help improving the microwave dielectric property of magnesium titanate ceramics.
Summary of the invention
The purpose of this invention is to provide a kind of effect of farthest bringing into play sintering aid, when a little auxiliary is added, can effectively reduce ceramics component of magnesium titanate ceramics sintering temperature and preparation method thereof.
1, a kind of low-temperature sintering magnesium titanate ceramics, it is characterized in that: raw-material molfraction consists of:
100 parts of the compounds of titanium
85～99 parts of the compounds of magnesium
1～15 part of the compound of calcium
0.1～20 part of the compound of zinc
0.1～20 part of the compound of barium
1～20 part of tetraethoxy
5～50 parts of boric acid
The compound of described titanium is one or more in tetrabutyl titanate, tetraethyl titanate or the titanium tetrachloride; The compound of described magnesium is one or more in magnesium nitrate, magnesium acetate or the magnesium chloride; The compound of described calcium is one or more in nitrocalcite, calcium acetate or the calcium chloride; The compound of described zinc is one or more in zinc nitrate, zinc acetate or the zinc chloride; The compound of described barium is one or more in nitrate of baryta, barium acetate or the bariumchloride.
As preferably, above-mentioned a kind of low-temperature sintering magnesium titanate ceramics, raw-material molfraction consists of:
100 parts of the compounds of titanium
90～95 parts of the compounds of magnesium
4～8 parts of the compounds of calcium
1～5 part of the compound of zinc
1～10 part of the compound of barium
1～5 part of tetraethoxy
10～25 parts of boric acid.
As optimal selection, raw-material molfraction consists of in above-mentioned a kind of low-temperature sintering magnesium titanate ceramics:
100 parts of the compounds of titanium
90 parts of the compounds of magnesium
5 parts of the compounds of calcium
4 parts of the compounds of zinc
10 parts of the compounds of barium
5 parts of tetraethoxys
12 parts of boric acid.
A kind of preparation method of low-temperature sintering magnesium titanate ceramics is characterized in that: comprise the steps:
(1) with the compound dissolution of titanium in acetic acid, form the solution of 0.5～2.0mol/l;
(2) compound, the compound of calcium, the compound of zinc, the compound of barium, the boric acid with magnesium is dissolved in the dehydrated alcohol, form the solution of 1.0～3.0mol/l, add an amount of pH value conditioning agent simultaneously the pH value of mixing solutions is transferred to 4.0～6.0, then tetraethoxy is added and mixing and stirring;
(3) solution with above-mentioned steps (1) joins in the solution of step (2), extraordinarily goes into deionized water by 2～8 of tetraethoxy quality simultaneously, presses 1%～5% of titanium elements quality then and adds tensio-active agent, mixing and stirring;
(4) above-mentioned mixing solutions is placed 40～60 ℃ water-bath, until obtaining transparent gel;
(5) with above-mentioned gel in 80～100 ℃ baking oven dry 10～24 hours, put into the high alumina crucible then, calcine, obtain the ceramic powder of white at 650～850 ℃;
(6) above-mentioned ceramic powder is carried out ball milling, add polyvinyl alcohol water solution then, and, carry out sintering, obtain the low-temperature sintering magnesium titanate ceramics at 890～1100 ℃ by behind granulation, moulding, the binder removal as tackiness agent;
Described pH value conditioning agent is one or more in nitric acid, hydrochloric acid or the acetic acid; Described tensio-active agent is one or more in oleic acid, polyoxyethylene glycol, polyvinyl alcohol or the polyvinyl butyral acetal.
As preferably, the compound dissolution of titanium forms the solution of 1.5～1.8mol/l in above-mentioned preparation method's the step (1) in acetic acid.
As preferably, compound, the compound of calcium, the compound of zinc, the compound of barium, boric acid with magnesium in above-mentioned preparation method's the step (2) are dissolved in the dehydrated alcohol, form the solution of 1.5～2.0mol/l, the pH value with mixing solutions transfers to 4.3～5.0 simultaneously.
As preferably, the quality that adds deionized water in above-mentioned preparation method's step (3) is 3～4 times of tetraethoxy, press 2%～3% adding tensio-active agent of titanium elements quality then.
The present invention compared with prior art, has following advantage: by the homodisperse of various starting material under solution state, realize magnesium titanate body material and sintering aid component uniform mixing in the atom level level, thereby can bring into play the effect of sintering aid to greatest extent, reduce the sintering aid consumption, reduce the negative impact of sintering aid the magnesium titanate ceramics dielectric properties; After 650～850 ℃ of calcinings, will obtain particle diameter at submicron even nano level superfine ceramic powder, utilize superfine powder high-ratio surface can with the synergy of sintering aid, under a small amount of sintering aid adds, reduce the sintering temperature of magnesium titanate ceramics as far as possible.
Embodiment
Below in conjunction with example the present invention is further described.
Embodiment 1:
Take by weighing 100 parts of tetrabutyl titanates and be dissolved in acetic acid, form the solution of 1.5mol/l.Taking by weighing 95 parts of magnesium nitrates, 5 parts of nitrocalcite, 1 part of zinc nitrate, 1 part of nitrate of baryta, 10 parts of boric acid is dissolved in the dehydrated alcohol, form the solution of 2.0mol/l, add 0.01 part of concentration simultaneously and be 5% nitric acid the pH value of solution is transferred to 4.5, add 1 part of tetraethoxy then, mix and stir the acetum that the back adds the tetrabutyl titanate that has prepared.In above-mentioned mixing solutions, add 2 parts of deionized waters and 5 parts of oleic acid, mixing and stirring.Above-mentioned mixing solutions is placed 60 ℃ water-bath, obtain clear gel; With above-mentioned gel in 90 ℃ baking oven dry 18 hours, put into the high alumina crucible then, 700 ℃ of calcinings 2 hours, obtain the ceramic powder of white.Above-mentioned ceramic powder is carried out ball milling, add 15 parts of polyvinyl alcohol water solutions then as tackiness agent, carry out granulation behind the thorough mixing, then at the forming under the pressure of 120Mpa, carry out sintering at 1100 ℃ behind the binder removal, promptly obtain low-temperature sintering magnesium titanate ceramics of the present invention.
Embodiment 2:
Take by weighing 100 parts of tetraethyl titanates and be dissolved in acetic acid, form the solution of 2.0mol/l.Taking by weighing 90 parts of magnesium acetates, 4.5 parts of calcium acetates, 3 parts of zinc acetates, 3 parts of barium acetates, 8 parts of boric acid is dissolved in the dehydrated alcohol, form the solution of 1.5mol/l, add 5 parts of acetic acid simultaneously the pH value of solution is transferred to 5.0, add 5 parts of tetraethoxys then, mix and stir the acetum that the back adds the tetraethyl titanate that has prepared.In above-mentioned mixing solutions, add 10 parts of deionized waters and 3 parts of polyoxyethylene glycol, mixing and stirring.Above-mentioned mixing solutions is placed 60 ℃ water-bath, obtain clear gel; With above-mentioned gel in 95 ℃ baking oven dry 12 hours, put into the high alumina crucible then, 750 ℃ of calcinings 2 hours, obtain the ceramic powder of white.Above-mentioned ceramic powder is carried out ball milling, add 16 parts of polyvinyl alcohol water solutions then as tackiness agent, carry out granulation behind the thorough mixing, then at the forming under the pressure of 120Mpa, carry out sintering at 1000 ℃ behind the binder removal, promptly obtain low-temperature sintering magnesium titanate ceramics of the present invention.
Embodiment 3:
Take by weighing 70 parts of tetrabutyl titanates and 30 parts of titanium tetrachlorides are dissolved in acetic acid, form the solution of 1.5mol/l.Taking by weighing 70 parts of magnesium nitrates, 22 parts of magnesium chlorides, 4 parts of nitrocalcite, 0.7 part of calcium chloride, 10 parts of zinc nitrates, 10 parts of zinc chloride, 10 parts of nitrate of baryta, 10 parts of bariumchlorides, 50 parts of boric acid is dissolved in the dehydrated alcohol, form the solution of 3.0mol/l, add 0.01 part of concentration simultaneously and be 5% nitric acid and 0.01 part of concentration and be 5% hydrochloric acid the pH value of solution is transferred to 4.3, add 20 parts of tetraethoxys then, mix and stir the acetum that the back adds the titanium compound that has prepared.In above-mentioned mixing solutions, add 40 parts of deionized waters and 5 parts of polyvinyl butyral acetals, mixing and stirring.Above-mentioned mixing solutions is placed 60 ℃ water-bath, obtain clear gel; With above-mentioned gel in 85 ℃ baking oven dry 24 hours, put into the high alumina crucible then, 720 ℃ of calcinings 2 hours, obtain the ceramic powder of white.Above-mentioned ceramic powder is carried out ball milling, add 20 parts of polyvinyl alcohol water solutions then as tackiness agent, carry out granulation behind the thorough mixing, then at the forming under the pressure of 120Mpa, carry out sintering at 900 ℃ behind the binder removal, promptly obtain low-temperature sintering magnesium titanate ceramics of the present invention.
Claims (7)
1. low-temperature sintering magnesium titanate ceramics, it is characterized in that: raw-material molfraction consists of:
100 parts of the compounds of titanium
85～99 parts of the compounds of magnesium
1～15 part of the compound of calcium
0.1～20 part of the compound of zinc
0.1～20 part of the compound of barium
1～20 part of tetraethoxy
5～50 parts of boric acid
The compound of described titanium is one or more in tetrabutyl titanate, tetraethyl titanate or the titanium tetrachloride; The compound of described magnesium is one or more in magnesium nitrate, magnesium acetate or the magnesium chloride; The compound of described calcium is one or more in nitrocalcite, calcium acetate or the calcium chloride; The compound of described zinc is one or more in zinc nitrate, zinc acetate or the zinc chloride; The compound of described barium is one or more in nitrate of baryta, barium acetate or the bariumchloride.
2. a kind of low-temperature sintering magnesium titanate ceramics according to claim 1, it is characterized in that: raw-material molfraction consists of:
100 parts of the compounds of titanium
90～95 parts of the compounds of magnesium
4～8 parts of the compounds of calcium
1～5 part of the compound of zinc
1～10 part of the compound of barium
1～5 part of tetraethoxy
10～25 parts of boric acid.
3. a kind of low-temperature sintering magnesium titanate ceramics according to claim 2, it is characterized in that: raw-material molfraction consists of:
100 parts of the compounds of titanium
90 parts of the compounds of magnesium
5 parts of the compounds of calcium
4 parts of the compounds of zinc
10 parts of the compounds of barium
5 parts of tetraethoxys
12 parts of boric acid.
4. the preparation method of a low-temperature sintering magnesium titanate ceramics is characterized in that: comprise the steps:
(1) with the compound dissolution of titanium in acetic acid, form the solution of 0.5～2.0mol/l;
(2) compound, the compound of calcium, the compound of zinc, the compound of barium, the boric acid with magnesium is dissolved in the dehydrated alcohol, form the solution of 1.0～3.0mol/l, add an amount of pH value conditioning agent simultaneously the pH value of mixing solutions is transferred to 4.0～6.0, then tetraethoxy is added and mixing and stirring;
(3) solution with above-mentioned steps (1) joins in the solution of step (2), extraordinarily goes into deionized water by 2～8 of tetraethoxy quality simultaneously, presses 1%～5% of titanium elements quality then and adds tensio-active agent, mixing and stirring;
(4) above-mentioned mixing solutions is placed 40～60 ℃ water-bath, until obtaining transparent gel;
(5) with above-mentioned gel in 80～100 ℃ baking oven dry 10～24 hours, put into the high alumina crucible then, calcine, obtain the ceramic powder of white at 650～850 ℃;
(6) above-mentioned ceramic powder is carried out ball milling, add polyvinyl alcohol water solution then, and, carry out sintering, obtain the low-temperature sintering magnesium titanate ceramics at 890～1100 ℃ by behind granulation, moulding, the binder removal as tackiness agent;
Described pH value conditioning agent is one or more in nitric acid, hydrochloric acid or the acetic acid; Described tensio-active agent is one or more in oleic acid, polyoxyethylene glycol, polyvinyl alcohol or the polyvinyl butyral acetal.
5. a kind of preparation method according to claim 4, the compound dissolution that it is characterized in that titanium in the described step (1) forms the solution of 1.5～1.8mol/l in acetic acid.
6. a kind of preparation method according to claim 4, it is characterized in that in the described step (2) compound, the compound of calcium, the compound of zinc, the compound of barium, the boric acid of magnesium are dissolved in the dehydrated alcohol, form the solution of 1.5～2.0mol/l, the pH value with mixing solutions transfers to 4.3～5.0 simultaneously.
7. a kind of preparation method according to claim 4, the quality that it is characterized in that adding deionized water in the described step (3) is 3～4 times of tetraethoxy, presses 2%～3% of titanium elements quality then and adds tensio-active agent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193488A (en) * | 2013-04-01 | 2013-07-10 | 漳州师范学院 | High-temperature resistant ceramic antibacterial agent coated with inorganic nano-material and preparation technology of high-temperature resistant ceramic antibacterial agent |
| CN104445231A (en) * | 2014-11-27 | 2015-03-25 | 中国计量学院 | Silicate nanometer powder with lower sintering temperature and preparation method thereof |
| CN111875372A (en) * | 2020-08-12 | 2020-11-03 | 广东国华新材料科技股份有限公司 | Microwave dielectric ceramic and preparation method thereof |
| CN114195510A (en) * | 2021-12-28 | 2022-03-18 | 元颉新材料科技(浙江)有限公司 | Pure crystalline phase high-quality factor nano-size magnesium calcium titanate ceramic powder and preparation method thereof |
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|---|---|---|---|---|
| CN1126709A (en) * | 1994-06-22 | 1996-07-17 | 三菱麻铁里亚尔株式会社 | Magnesia-titania refractory and method for manufacturing the same |
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2010
- 2010-09-30 CN CN2010102984558A patent/CN102030525B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1126709A (en) * | 1994-06-22 | 1996-07-17 | 三菱麻铁里亚尔株式会社 | Magnesia-titania refractory and method for manufacturing the same |
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of the European Ceramic Society》 20001231 Heli Jantunen et.al. Compositions of MgTiO3-CaTiO3 ceramic with two borosilicate glasses for LTCC technology 2331-2336 1-7 第20卷, 第14-15期 * |
| 《硅酸盐通报》 20070630 王加芳，罗驹华 纳米钛酸镁陶瓷粉体的制备研究进展 514-518，546 1-7 第26卷, 第3期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193488A (en) * | 2013-04-01 | 2013-07-10 | 漳州师范学院 | High-temperature resistant ceramic antibacterial agent coated with inorganic nano-material and preparation technology of high-temperature resistant ceramic antibacterial agent |
| CN104445231A (en) * | 2014-11-27 | 2015-03-25 | 中国计量学院 | Silicate nanometer powder with lower sintering temperature and preparation method thereof |
| CN104445231B (en) * | 2014-11-27 | 2016-06-29 | 中国计量学院 | A kind of silicate nano powder body with lower sintering temperature and preparation method thereof |
| CN111875372A (en) * | 2020-08-12 | 2020-11-03 | 广东国华新材料科技股份有限公司 | Microwave dielectric ceramic and preparation method thereof |
| CN114195510A (en) * | 2021-12-28 | 2022-03-18 | 元颉新材料科技(浙江)有限公司 | Pure crystalline phase high-quality factor nano-size magnesium calcium titanate ceramic powder and preparation method thereof |
| CN114195510B (en) * | 2021-12-28 | 2024-04-23 | 元颉新材料科技(浙江)有限公司 | Pure crystal phase high-quality factor nano-sized magnesium calcium titanate ceramic powder and preparation method thereof |
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