CN109081691A - A kind of tubular ceramic preparation method - Google Patents

A kind of tubular ceramic preparation method Download PDF

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Publication number
CN109081691A
CN109081691A CN201811068122.9A CN201811068122A CN109081691A CN 109081691 A CN109081691 A CN 109081691A CN 201811068122 A CN201811068122 A CN 201811068122A CN 109081691 A CN109081691 A CN 109081691A
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China
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column
quality
ceramic
barium
strontium
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CN201811068122.9A
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CN109081691B (en
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赵鹏
李卓
景明海
苏兴华
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Changan University
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Changan University
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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
    • C04B35/468Shaped 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 barium 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
    • 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
    • C04B35/64Burning or sintering processes
    • 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
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213Strontium oxides or oxide-forming salts thereof

Abstract

The invention discloses a kind of tubular ceramic preparation methods.Disclosed method includes: to shape after addition adhesive by after ceramic powder pre-burning and obtain column;Preference temperature, suitable column radial section size of current are suitable for being sintered under conditions of being sintered duration to column, so that generating the loose cylinder outside formation quality densification tube body of the loose cylinder of quality, quality partially along axial in column;It rejects the loose cylinder of quality and obtains tubular ceramic.The present invention by controlling electric sintering condition that burning occurs among ceramics sample, directly in ceramic densifying engineering, forms hollow structure;Gained tubular electron ceramic crystalline grain is small, and uniformly, dielectric properties are excellent.

Description

A kind of tubular ceramic preparation method
Technical field
The invention belongs to electron ceramic material preparation technical fields, and in particular to a kind of tubular ceramic preparation method.
Background technique
Power plant's assisted sintering technology is a kind of new ceramics sintering method occurred in recent years.Earliest comes across nineteen fifty-two In the article of Hill, electric current is directly passed through the cermet being brought rapidly up under pressure subsidiary conditions by described in the text one kind Green body, the method to prepare cermet block materials.Now described flash burning is a new sintering concept, 2010 by The report such as Cologna, zirconium oxide [3% (molar fraction) Y2O3-ZrO2, the 3YSZ] pottery in this text and its subsequent research paper Porcelain blank sintering obtains well as a result, still insulator electric current sintering relative difficulty is some.
Tubular electron ceramics belong to hollow structure, and special mold is needed to carry out pressure forming, and in the densification sintered Aperture in ceramic body needs to laser machine, time-consuming and laborious.
Summary of the invention
It is for the defects in the prior art and insufficient, a kind of tubular ceramic preparation method of the present invention
Tubular ceramic preparation method provided by the invention includes: to shape after ceramic powder pre-burning after addition adhesive Obtain column;Preference temperature, be suitable for column radial section size of current, be suitable under conditions of being sintered duration to column into Row is sintered, so that partially along formation quality densification pipe outside the loose cylinder of axial generation quality, the loose cylinder of quality in column Body;It rejects the loose cylinder of quality and obtains tubular ceramic.
Further, the column is cylindrical body.
Optionally, the electric current is alternating current or DC current.
Further, the present invention also provides a kind of tubulose barium-strontium titanate ceramic preparation methods.Provided tubulose strontium titanates Titanate ceramics preparation method includes:
After strontium-barium titanate ceramic powder pre-burning, forming obtains column after adding adhesive;700-1000 DEG C, column Body radial section electric current is is sintered 0.5-10 minutes to column under conditions of 10-50 milliamperes/square millimeter, part in column Quality densification tube body is formed along the axial loose cylinder outside of the loose cylinder of quality, quality that generates;The loose cylinder of quality is rejected to obtain Tubulose barium-strontium titanate ceramic.
Preferably, strontium atom molal quantity accounts for the 15%-85% of strontium barium atom total mole number in the barium-strontium titanate ceramic; The binder is PVA, and the binder accounts for the 0.8%-1.2% of the barium-strontium titanate powder quality, and the calcined temperature is 900-1100℃。
Advantages of the present invention are as follows:
(1) present invention by controlling electric sintering condition that burning occurs among ceramics sample, directly in ceramic densifying In engineering, hollow structure is formed.
(2) tubular electron ceramic crystalline grain of the invention is small, and uniformly, dielectric properties are excellent.
Detailed description of the invention
Fig. 1 is the dielectric properties curve of 1 gained tubular ceramic material of embodiment.
Fig. 2 is 1 gained column structure schematic diagram of embodiment.
Specific embodiment
Technique of the invention is suitable for the preparation of tubular ceramic material, below to the present invention for selection barium-strontium titanate ceramic It is further explained explanation.For other types ceramics, thinking according to the present invention selects suitable temperature, electric current, burning Ceramic tube can be obtained in knot duration, can also formula to ceramic material and pre-burning link carry out selectivity optimization and obtain tubular ceramic material Material.
Embodiment 1:
According to barium strontium molar ratio be 7:3 strontium-barium titanate ceramic powder 1000 DEG C at a temperature of pre-burning 2 hours after, add The PVA adhesive for adding 1%, 200Mpa forming under the pressure at 6 millimeters of diameter, cylindrical body that length is 3 millimeters;In cylindrical body Upper application voltage, total current control within the scope of 300 milliamperes, are sintered 300 seconds under 970 DEG C of furnace temperature and obtain column as shown in Figure 2 Body;As shown in Fig. 2, gained sintering column internal cause burning generation crystal grain powder is excessive, the loose column of quality without mechanical strength Body (black lines identified areas in figure), it can be seen from the figure that the color of the loose column of the quality is compared with periphery dense material It is of light color, close to white, reject after the loose column of part quality to obtain tubular ceramic using mechanical or laser means.- It is as shown in table 1 to measure tubular electron ceramic dielectric performance for dielectric and magnetic sweep check at a temperature of 30 DEG C -140 DEG C.Its dielectricity Energy curve is as shown in Figure 1.
Table 1
Maximum dielectric constant Loss angle tangent Curie point
11766 0.08425 6.0
Embodiment 2:
According to barium strontium than the strontium-barium titanate ceramic powder for 8:2 1100 DEG C at a temperature of pre-burning 1 hour after, addition 1% PVA adhesive, 300Mpa forming under the pressure at 6 millimeters of diameter, cylindrical body that length is 3 millimeters;Apply DC voltage, Current control is sintered 400 seconds under 700 DEG C of furnace temperature within the scope of 1000 milliamperes;Middle part is rejected using mechanical or laser means Sub-prime after loose column tubular ceramic.- 30 DEG C -140 DEG C at a temperature of measure tubular electron ceramic dielectric performance such as Shown in table 2.
Table 2
Maximum dielectric constant Loss angle tangent Curie point oC
10621 0.00353 9.0
Embodiment 3:
According to barium strontium than the strontium-barium titanate ceramic powder for 1:1 900 DEG C at a temperature of pre-burning 2 hours after, addition 1.2% PVA adhesive, 300Mpa forming under the pressure at 6 millimeters of diameter, cylindrical body that length is 3 millimeters;Using silver electrode, Apply DC voltage, current control is sintered 400 seconds under 850 DEG C of furnace temperature within the scope of 600 milliamperes;Using mechanical or laser hand Section obtains tubular ceramic after rejecting the loose column of middle section quality.- 30 DEG C -140 DEG C at a temperature of measure tubular electron pottery Porcelain dielectric properties are as shown in table 3.
Table 3
Maximum dielectric constant Loss angle tangent Curie point
8162 0.05502 3.8

Claims (5)

1. a kind of tubular ceramic preparation method, which is characterized in that method includes:
After ceramic powder pre-burning, is shaped after addition adhesive and obtain column;
Preference temperature, is suitable for being sintered under conditions of being sintered duration to column at suitable column radial section size of current, So that forming quality densification tube body partially along the axial loose cylinder outside of the loose cylinder of quality, quality that generates in column;
It rejects the loose cylinder of quality and obtains tubular ceramic.
2. tubular ceramic preparation method as described in claim 1, which is characterized in that the column is cylindrical body.
3. tubular ceramic preparation method as described in claim 1, which is characterized in that the electric current is alternating current or direct current Electric current.
4. a kind of tubulose barium-strontium titanate ceramic preparation method, which is characterized in that method includes:
After strontium-barium titanate ceramic powder pre-burning, forming obtains column after adding adhesive;
700-1000 DEG C, column radial section electric current be 10-50 milliampere/square millimeter under conditions of to column sintering 0.5- 10 minutes, column is interior to form quality densification tube body partially along the axial loose cylinder outside of the loose cylinder of quality, quality that generates;
It rejects the loose cylinder of quality and obtains tubulose barium-strontium titanate ceramic.
5. tubulose barium-strontium titanate ceramic preparation method as claimed in claim 4, which is characterized in that method includes: the metatitanic acid Strontium atom molal quantity accounts for the 15%-85% of strontium barium atom total mole number in strontium titanate ceramics;The binder is PVA, the bonding Agent accounts for the 0.8%-1.2% of the barium-strontium titanate powder quality, and the calcined temperature is 900-1100 DEG C.
CN201811068122.9A 2018-09-13 2018-09-13 Tubular ceramic preparation method Expired - Fee Related CN109081691B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111261935A (en) * 2020-03-04 2020-06-09 四川固蜀材料科技有限公司 Sodium ion conductor solid electrolyte material, preparation method and application
CN115304369A (en) * 2022-03-09 2022-11-08 陕西科技大学 Preparation method of high-dielectric high-breakdown strontium titanate ceramic

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86103814A (en) * 1985-04-25 1987-03-04 谭氏陶器有限公司 Ultra-low fire ceramic composition
JP2000239708A (en) * 1999-02-16 2000-09-05 Ishikawajima Harima Heavy Ind Co Ltd Sintering device
CN204993912U (en) * 2015-07-23 2016-01-20 张贻新 Energy -conserving ceramic electrothermal tube
CN109357528A (en) * 2018-08-14 2019-02-19 长安大学 A kind of ceramic material sintering furnace and its control method using electric field-assisted

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86103814A (en) * 1985-04-25 1987-03-04 谭氏陶器有限公司 Ultra-low fire ceramic composition
JP2000239708A (en) * 1999-02-16 2000-09-05 Ishikawajima Harima Heavy Ind Co Ltd Sintering device
CN204993912U (en) * 2015-07-23 2016-01-20 张贻新 Energy -conserving ceramic electrothermal tube
CN109357528A (en) * 2018-08-14 2019-02-19 长安大学 A kind of ceramic material sintering furnace and its control method using electric field-assisted

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111261935A (en) * 2020-03-04 2020-06-09 四川固蜀材料科技有限公司 Sodium ion conductor solid electrolyte material, preparation method and application
CN115304369A (en) * 2022-03-09 2022-11-08 陕西科技大学 Preparation method of high-dielectric high-breakdown strontium titanate ceramic
CN115304369B (en) * 2022-03-09 2023-08-22 陕西科技大学 Preparation method of high-dielectric high-breakdown strontium titanate ceramic

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