CN108129146A - A kind of high dielectric constant and low dielectric loss strontium titanate ceramics - Google Patents

A kind of high dielectric constant and low dielectric loss strontium titanate ceramics Download PDF

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CN108129146A
CN108129146A CN201810058238.8A CN201810058238A CN108129146A CN 108129146 A CN108129146 A CN 108129146A CN 201810058238 A CN201810058238 A CN 201810058238A CN 108129146 A CN108129146 A CN 108129146A
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ceramics
ball
powder
dielectric loss
strontium titanate
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李蔚
傅文平
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East China University of Science and Technology
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East China University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/465Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C04B35/47Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on strontium titanates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/6261Milling
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof

Abstract

The present invention discloses a kind of high-k, low-dielectric loss strontium titanates(SrTiO3)The preparation method of ceramics, main technical schemes are:First with SrCO3、TiO2And Nb2O5For raw material, by by chemical formula SrTi(1‑1.25x)Nb x O3Feeding is matched, dry powder is obtained after wet ball grinding is mixed, dried, dry powder is placed in electric furnace after calcining appropriate time at a certain temperature and taken out, then after wet ball grinding, drying, sieving, you can obtain thin strontium titanate ceramic powder;By powder it is dry-pressing formed after, be placed in high-temperature electric resistance furnace, under conditions of 1,420 1480 DEG C be sintered 2h obtain required strontium titanate ceramics.The strontium titanate ceramics that the present invention is obtained have excellent dielectric properties, and medium dielectric constant microwave medium can maintain 296 303, suitable with common strontium titanate ceramics, and Q ×fClose to 7000GHz when being worth highest, far above common strontium titanate ceramics.Present invention process is simple, is easy to large-scale production, has very high practical value.

Description

A kind of high dielectric constant and low dielectric loss strontium titanate ceramics
Technical field
The present invention relates to a kind of high dielectric constant and low dielectric loss strontium titanates(SrTiO3)Ceramics belong to microwave dielectric material Field, available for communicating, the fields such as radar, electronics.
Background technology
In recent years, as short-wave communication tedhnology development is getting faster, increasingly higher demands are proposed to microwave dielectric material. In general, microwave dielectric material must have high dielectric constant(εr), high Q ×fValue and near-zero frequency temperature coefficient (τ f ).Strontium titanate ceramics have very high permittivity εr(~300)Very big positive temperature coefficient τ f + 1100ppm/ DEG C of ≈, can With some low-ks, the Material cladding of negative temperature coefficient, the microwave dielectric material of function admirable is obtained.Such as Huang is adopted Use SrTiO3With negative frequency temperature coefficient(τ f ≈-42×10-6/℃)Nd (Zn1/2Ti1/2)O3Compound, obtaining dielectric constant is 54.2, Q ×fIt is 84,000GHz to be worth, temperature coefficient τ f ≈0×10-6/ DEG C (1x)Nd(Zn1/2Ti1/2)O3xSrTiO3It is compound Ceramics(x=When 0.52);Wang etc. has foundxSrTiO3– (1-x)Ca(Mg1/3Nb2/3)O3In system, whenxIt is compound when=0.3 Ceramics dielectric constant (ε r ) for 46, Q ×fIt is worth for 29,300GHz, τ f ≈-2×10-6/℃;GONG etc. also once worked as by reportx= When 0.02, (1-x)MgSn0.05Ti0.95O3-xSrTiO3Composite ceramic material has very excellent dielectric properties(ε r =19.32 Q ×fIt is worth for 193.527 THz, τ f =2×10-6/℃).But, since strontium titanate ceramics dielectric loss is larger, Q ×fValue is not high (~1000GHz), can have to the further reduction of its dielectric loss with other materials after compound and have an adverse effect.Therefore it drops The dielectric loss of low strontium titanate ceramics, improve its own Q ×fIt is worth necessary.Strontium titanate ceramics are carried out with appropriate doping Be it is a kind of raising its Q ×fThe common methods of value, but dopant or doping way select not at that time, to frequently can lead to dielectric Constant declines, this is equally unfavorable for the application of strontium titanate ceramics.Therefore, how to be improved on the basis of the decline of dielectric constant unobvious The Q of strontium titanate ceramics ×fValue, is a urgent and significant subject.
Invention content
Present invention aims at a kind of method for preparing high-k, low-dielectric loss strontium titanate ceramics is provided, solve Strontium titanate ceramics dielectric loss in the prior art(tanδ)Higher, Q ×fIt is worth the problem of relatively low.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is as follows:First with SrCO3、TiO2And Nb2O5 For raw material, after preparing according to a certain ratio, mixture is obtained after wet ball grinding is mixed, dried, mixture is placed in electric furnace, It is taken out after calcining appropriate time under certain temperature, then thin strontium titanate ceramics powder is can obtain after wet ball grinding, drying and screening Body;By gained powder it is dry-pressing formed after, be placed in high-temperature electric resistance furnace under conditions of 1420-1480 DEG C be sintered 2-3h obtain it is required Strontium titanate ceramics.
In the technical scheme, SrCO3、TiO2And Nb2O5Consumption proportion press chemical formula SrTi(1-1.25x)Nb x O3It calculates, WhereinxValue is 0.002-0.005.During mixing ball-milling medium be zirconia ball and water, ball:Water:Expect to be 2:2:1, incorporation time For 20-30h.Mixture drying temperature is 80-120 DEG C, and calcination temperature is 1100-1200 DEG C, calcination time 2-5h.It calcines Sr titanate powder again ball milling when ball-milling medium for zirconia ball and water, ball:Water:Expect to be 3:2:1, Ball-milling Time 20- 30h, powder drying temperature is 80-120 DEG C after ball milling, and the powder after drying crosses grit number as 40 mesh.Dry-pressing formed pressure is 100-150MPa, blank sintering temperature are 1420-1480 oC, soaking time 2-3h.
The strontium titanate ceramics that the present invention is obtained have excellent dielectric properties, and medium dielectric constant microwave medium can maintain 296- 303, it will not be with Nb2O5The variation of doping and be decreased obviously, and Q ×fValue is then with Nb2O5The increase of doping and by Step improves, close to 7000GHz during highest, far above 1000GHz of common strontium titanate ceramics or so.Present invention process is simple, easily In large-scale production, there is very high practical value.
Description of the drawings
Fig. 1 is that the present invention obtains Nb2O5The dielectric properties of strontium titanate doping ceramics sample.
Fig. 1 is used to provide further understanding of the present invention, and a part for constitution instruction, the implementation with the present invention Example for explaining the present invention, is not construed as limiting the invention together.
Specific embodiment
The preferred embodiment of the present invention is illustrated below in conjunction with attached drawing 1, it should be appreciated that described herein preferred Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the present invention.
Embodiment 1:A kind of high-k, low-dielectric loss strontium titanate ceramics, it is to be prepared by the following method 's:To analyze pure SrCO3、TiO2And Nb2O5For raw material, by chemical formula SrTi(1-1.25x)Nb x O3Proportioning calculates each raw material dosage(x 0,0.002,0.003,0.004,0.005 is taken respectively), it is placed in 5 ball grinders, it is ball to select zirconia ball and deionized water Grinding media carries out wet ball grinding, ball:Water:Expect to be 2:2:1, incorporation time is for 24 hours.It is taken out after powder mixing, in 100 DEG C of baking It is dried in case, then calcines 3h at 1150 DEG C.The Sr titanate powder calcined is taken out, then is respectively charged into 6 ball grinders Ball milling.Ball-milling medium be zirconia ball and deionized water, ball:Water:Expect to be 3:2:1, Ball-milling Time is for 24 hours.By powder after ball milling Take out drying, drying temperature be 100 DEG C, the powder after drying cross 40 mesh sieve, then under the pressure of 100MPa it is dry-pressing formed into The cylindrical sample of diameter about 16mm, height about 12mm, are placed in Muffle furnace, 4h are kept the temperature at 1450 DEG C.
The sample baked is taken out, utilizes the dielectric properties of Hakii-Coleman dielectric posts Dissipative Resistance by Harmonic Resonance Method test agents, knot Fruit shows as shown in Figure 1:Work as Nb2O5Doping the dielectric properties of strontium titanate ceramics are had not significant impact, and Q ×fValue with Nb2O5Doping step up, as x=0.005, Q ×fValue reaches highest, is 6953GHz, at this time dielectric constant It is 296.

Claims (7)

1. a kind of high-k, low-dielectric loss strontium titanates(SrTiO3)Ceramics, basic technology are:First with SrCO3、 TiO2And Nb2O5For raw material, after preparing according to a certain ratio, dry powder is obtained after wet ball grinding is mixed, dried, dry powder is placed in electricity It is taken out after calcining appropriate time at a certain temperature in stove, then thin strontium titanates is can obtain after wet ball grinding, drying and screening Ceramic powder;By powder it is dry-pressing formed after, be placed in high-temperature electric resistance furnace, be sintered under conditions of 1420-1480 DEG C needed for 2h obtains Strontium titanate ceramics.
2. a kind of high-k, low-dielectric loss strontium titanates according to claim 1(SrTiO3)Ceramics, it is characterised in that: In the technical scheme, SrCO3、TiO2And Nb2O5Consumption proportion press chemical formula SrTi(1-1.25x)Nb x O3It calculates, whereinxValue For 0.002-0.005.
3. a kind of high-k, low-dielectric loss strontium titanates according to claim 1(SrTiO3)Ceramics, it is characterised in that: During mixing ball-milling medium be zirconia ball and water, ball:Water:Expect to be 2:2:1, incorporation time 20-30h.
4. a kind of high-k, low-dielectric loss strontium titanates according to claim 1(SrTiO3)Ceramics, it is characterised in that: Mixed powder drying temperature is 80-120 DEG C, and powder calcination temperature is 1100-1200 DEG C, calcination time 2-5h.
5. a kind of high-k, low-dielectric loss strontium titanates according to claim 1(SrTiO3)Ceramics, it is characterised in that: Calcined powder again ball milling when ball-milling medium for zirconia ball and water, ball:Water:Expect to be 3:2:1, Ball-milling Time 20-30h.
6. a kind of high-k, low-dielectric loss strontium titanates according to claim 1(SrTiO3)Ceramics, it is characterised in that: Powder drying temperature is 80-120 DEG C after ball milling, and the powder after drying crosses grit number as 40 mesh.
7. a kind of high-k, low-dielectric loss strontium titanates according to claim 1(SrTiO3)Ceramics, it is characterised in that: Dry-pressing formed pressure is 100-150MPa, and blank sintering temperature is 1420-1480 oC, soaking time 2h.
CN201810058238.8A 2018-01-22 2018-01-22 A kind of high dielectric constant and low dielectric loss strontium titanate ceramics Pending CN108129146A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117051369A (en) * 2023-10-11 2023-11-14 北京航空航天大学宁波创新研究院 Preparation method of strontium niobate-doped target, target and magnetron sputtering film

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117051369A (en) * 2023-10-11 2023-11-14 北京航空航天大学宁波创新研究院 Preparation method of strontium niobate-doped target, target and magnetron sputtering film
CN117051369B (en) * 2023-10-11 2024-01-05 北京航空航天大学宁波创新研究院 Preparation method of strontium niobate-doped target, target and magnetron sputtering film

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