CN107721434A - Suitable for the piezo-electric ceramic composite material preparation method of transformer - Google Patents
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- CN107721434A CN107721434A CN201711122397.1A CN201711122397A CN107721434A CN 107721434 A CN107721434 A CN 107721434A CN 201711122397 A CN201711122397 A CN 201711122397A CN 107721434 A CN107721434 A CN 107721434A
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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Abstract
The invention discloses the piezo-electric ceramic composite material preparation method suitable for transformer, this method, which uses, to carry out ball-milling treatment after silicon nitride, aluminum oxide, silver vanadate mixing, ball-milled mixtures are placed in ethylene glycol, add tetraethyl orthosilicate, m-phenylene diamine (MPD), polyaluminosiloxane, agitating and heating obtains thermal response mixed liquor, again by dry ceramic slurry after thermal response mixed liquor ripening, regulation pH, finally ceramic slurry is solidified in a mold, is stripped, blank is obtained, then blank is sintered to the piezo-electric ceramic composite material that must be applied to transformer.The piezo-electric ceramic composite material suitable for transformer being prepared, it is not leaded, and mechanical strength and compressive resistance are high, have preferable application prospect in electronic device product.
Description
Technical field
The present invention relates to this technical field of electronic material, is related specifically to the piezoelectric ceramics composite wood suitable for transformer
Preparation method for material.
Background technology
Piezoelectric is a kind of new function material that can carry out energy conversion, and it can be realized between mechanical energy and electric energy
Conversion, with the fast development of electronics technology and information technology, piezoelectric is more and more general in the every field that people live
Time.
Piezoelectric ceramics is a kind of typical dielectric substance, and polarization can be produced in the presence of electric field or polarized state changes
Become, inductively transmit the effect of electricity, it is widely used in the neck such as aerospace, electronics, computer, ultrasound, laser and energy
Domain.With the development of modern science and technology, the application of power-type piezoelectric ceramics is increasingly extensive.Such as the piezoelectricity developed rapidly in recent years
Motor, piezoelectric actuator, Piezoelectric Vibration Feeder, all kinds of piezoelectric transformers, large power supersonic welding and be cleaned by ultrasonic and
Underwater acoustic transducer applied to national defence etc. is all based on high-performance high power piezoelectric ceramic material, and these applications are to piezoelectricity
Ceramic material proposes higher requirement.Wherein for its widely used field transformer, traditional transformer material
It is poor to there is even compact, mechanical strength is low, and piezoelectric activity is undesirable, and energy consumption is big, cost is high, lead volatility is made during high temperature sintering
Into environmental pollution and component deviation and piezoelectric property is influenceed, the deficiency of the reduction of piezoelectric property is caused in low-temperature sintering.
The content of the invention
In order to solve the above technical problems, the present invention provides the piezo-electric ceramic composite material preparation method suitable for transformer,
This method, which is used, to carry out ball-milling treatment after silicon nitride, aluminum oxide, silver vanadate mixing, and ball-milled mixtures are placed in ethylene glycol,
Tetraethyl orthosilicate, m-phenylene diamine (MPD), polyaluminosiloxane are added, agitating and heating obtains thermal response mixed liquor, then by thermal response mixed liquor
Dry ceramic slurry after ripening, regulation pH, ceramic slurry is finally solidified, be stripped in a mold, obtains blank, then will
Blank sinters the piezo-electric ceramic composite material that must be applied to transformer.The piezoelectric ceramics suitable for transformer being prepared is compound
Material, it is not leaded, and mechanical strength and compressive resistance are high, have preferable application prospect in electronic device product.
The purpose of the present invention can be achieved through the following technical solutions:
Suitable for the piezo-electric ceramic composite material preparation method of transformer, comprise the following steps:
(1)Silicon nitride 50-60 parts, aluminum oxide 25-35 parts, silver vanadate 10-20 parts are mixed, are put into ball-milling treatment in ball mill,
Obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add tetraethyl orthosilicate 12-18 parts, m-phenylene diamine (MPD) 8-12 parts, PVC insulated nylon sheathed building wire
Oxygen alkane 3-5 parts, 150 DEG C are heated to while stirring, keep 30 min, obtain thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould and solidified, then the demoulding, obtains blank, blank then is sent into sintering furnace,
It is sintered at 1300-1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
Preferably, the step(1)Middle ball-milling treatment is the h of ball milling 3 under rotating speed 220-250 r/min.
Preferably, the step(4)Solidification is that 60-80 min are carried out under the conditions of 250 DEG C, 15MPa.
Preferably, the step(4)In, it will be first sintered again after blank pre-burning, calcined temperature is 950 DEG C, during pre-burning
Between be 1.5 h.
Compared with prior art, its advantage is the present invention:
(1)The preparation method of the piezo-electric ceramic composite material suitable for transformer of the present invention is used silicon nitride, aluminum oxide, vanadium
Ball-milling treatment is carried out after sour silver mixing, ball-milled mixtures are placed in ethylene glycol, add tetraethyl orthosilicate, m-phenylene diamine (MPD), poly-aluminium
Siloxanes, agitating and heating obtain thermal response mixed liquor, then by dry ceramic slurry after thermal response mixed liquor ripening, regulation pH
Material, ceramic slurry is finally solidified, be stripped in a mold, obtains blank, then blank is sintered to the piezoelectricity that must be applied to transformer
Ceramic composite.The piezo-electric ceramic composite material suitable for transformer being prepared, it is not leaded, mechanical strength and pressure-resistant
Intensity is high, has preferable application prospect in electronic device product.
(2)Present invention employs silicon nitride, aluminum oxide, silver vanadate, tetraethyl orthosilicate, m-phenylene diamine (MPD), polyaluminosiloxane this
Several raw material compoundings prepare piezoceramic material, although these materials be not first Application in ceramic material, according to certain
After proportional quantity is applied in combination, it is aided with corresponding processing mode, is brought to the ceramic material being finally prepared in performance
Increase substantially, this is never to report in conventional research, for realize the present invention technique effect serve certainly
Qualitatively act on.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1)By 10 parts of 50 parts of silicon nitride, 25 parts of aluminum oxide, silver vanadate mixing, the ball under the r/min of rotating speed 220 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 12 parts of tetraethyl orthosilicate, 8 parts of m-phenylene diamine (MPD), polyaluminosiloxane 3
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 60 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1300 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
Embodiment 2
(1)By 15 parts of 55 parts of silicon nitride, 30 parts of aluminum oxide, silver vanadate mixing, the ball under the r/min of rotating speed 235 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 15 parts of tetraethyl orthosilicate, 10 parts of m-phenylene diamine (MPD), polyaluminosiloxane 4
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 70 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1400 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
Embodiment 3
(1)By 20 parts of 60 parts of silicon nitride, 35 parts of aluminum oxide, silver vanadate mixing, the ball under the r/min of rotating speed 250 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 18 parts of tetraethyl orthosilicate, 12 parts of m-phenylene diamine (MPD), polyaluminosiloxane 5
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 80 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
Comparative example 1
(1)By 20 parts of 60 parts of silicon nitride, 35 parts of aluminum oxide, barium nitrate mixing, the ball under the r/min of rotating speed 250 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 18 parts of tetraethyl orthosilicate, 12 parts of m-phenylene diamine (MPD), polyaluminosiloxane 5
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 80 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
Comparative example 2
(1)By 20 parts of 60 parts of silicon nitride, 35 parts of aluminum oxide, silver vanadate mixing, the ball under the r/min of rotating speed 250 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 18 parts of ethyl acetate, 12 parts of m-phenylene diamine (MPD), polyaluminosiloxane 5
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 80 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
Comparative example 3
(1)By 20 parts of 60 parts of silicon nitride, 35 parts of aluminum oxide, silver vanadate mixing, the ball under the r/min of rotating speed 250 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 18 parts of tetraethyl orthosilicate, 12 parts of ammonium persulfate, polyaluminosiloxane 5
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 80 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
Comparative example 4
(1)By 20 parts of 60 parts of silicon nitride, 35 parts of aluminum oxide, silver vanadate mixing, the ball under the r/min of rotating speed 250 is put into ball mill
3 h are ground, obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add 18 parts of tetraethyl orthosilicate, 12 parts of m-phenylene diamine (MPD), Polycarbosilane 5
Part, 150 DEG C are heated to while stirring, are kept 30 min, are obtained thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould under the conditions of 250 DEG C, 15MPa and carries out 80 min curing process, then the demoulding,
Blank is obtained, blank is then sent into sintering furnace pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h, then will be through pre-
The blank of burning is sintered at 1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
The performance test results of obtained piezoceramic material are as shown in table 1.
By embodiment 1-3 and comparative example 1-4 obtained piezoceramic material carry out respectively tensile strength, bending strength,
This several performance tests of compressive resistance.
Table 1
Tensile strength(MPa) | Bending strength(MPa) | Compressive resistance(KV/mm) | |
Embodiment 1 | 58.4 | 192.3 | 19.6 |
Embodiment 2 | 59.2 | 193.4 | 21.3 |
Embodiment 3 | 58.5 | 192.7 | 20.4 |
Comparative example 1 | 57.6 | 189.6 | 17.7 |
Comparative example 2 | 58.0 | 189.9 | 18.0 |
Comparative example 3 | 58.3 | 190.5 | 17.9 |
Comparative example 4 | 57.7 | 189.8 | 18.6 |
The preparation method of the piezo-electric ceramic composite material suitable for transformer of the present invention is used silicon nitride, aluminum oxide, vanadic acid
Ball-milling treatment is carried out after silver mixing, ball-milled mixtures are placed in ethylene glycol, adds tetraethyl orthosilicate, m-phenylene diamine (MPD), PVC insulated nylon sheathed building wire
Oxygen alkane, agitating and heating obtain thermal response mixed liquor, then by dry ceramic slurry after thermal response mixed liquor ripening, regulation pH
Material, ceramic slurry is finally solidified, is stripped, obtain blank, then blank is sintered to obtain into piezoceramic material in a mold.Prepare and
Into the piezo-electric ceramic composite material suitable for transformer, it is not leaded, and mechanical strength and compressive resistance are high, is produced in electronic device
There is preferable application prospect in product.Meanwhile the piezo-electric ceramic composite material raw material suitable for transformer of the invention is easy to get, work
Skill is simple, is used suitable for heavy industrialization, practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (4)
1. suitable for the piezo-electric ceramic composite material preparation method of transformer, it is characterised in that comprise the following steps:
(1)Silicon nitride 50-60 parts, aluminum oxide 25-35 parts, silver vanadate 10-20 parts are mixed, are put into ball-milling treatment in ball mill,
Obtain ball-milled mixtures;
(2)Ball-milled mixtures are placed in ethylene glycol, add tetraethyl orthosilicate 12-18 parts, m-phenylene diamine (MPD) 8-12 parts, PVC insulated nylon sheathed building wire
Oxygen alkane 3-5 parts, 150 DEG C are heated to while stirring, keep 30 min, obtain thermal response mixed liquor;
(3)Thermal response mixed liquor is aged 12 h at room temperature, adjusts pH to 8.0 with 3 mol/L sodium hydroxide solution, then
It is placed at 80 DEG C and dries 8 h, obtains ceramic slurry;
(4)Ceramic slurry is added in mould and solidified, then the demoulding, obtains blank, blank then is sent into sintering furnace,
It is sintered at 1300-1500 DEG C, is incubated 2 h, piezoceramic material is obtained after cooling to room temperature with the furnace.
2. the piezo-electric ceramic composite material preparation method according to claim 1 suitable for transformer, it is characterised in that
The step(1)Middle ball-milling treatment is the h of ball milling 3 under rotating speed 220-250 r/min.
3. the piezo-electric ceramic composite material preparation method according to claim 1 suitable for transformer, it is characterised in that institute
State step(4)Solidification is that 60-80 min are carried out under the conditions of 250 DEG C, 15MPa.
4. the piezo-electric ceramic composite material preparation method according to claim 1 suitable for transformer, it is characterised in that institute
State step(4)In, it will be first sintered again after blank pre-burning, calcined temperature is 950 DEG C, and burn-in time is 1.5 h.
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CN102093067A (en) * | 2010-12-14 | 2011-06-15 | 江苏联能电子技术有限公司 | Nano Al2O3 crystal whisker-toughened ceramic material with high piezoelectric property and preparation method thereof |
JP2013128006A (en) * | 2011-12-16 | 2013-06-27 | Ngk Insulators Ltd | Method for manufacturing piezoelectric/electrostrictive material film |
CN105254287A (en) * | 2015-09-29 | 2016-01-20 | 苏州宽温电子科技有限公司 | Nano piezoceramic material and preparation method thereof |
CN105272327A (en) * | 2015-09-29 | 2016-01-27 | 苏州宽温电子科技有限公司 | Whisker reinforced piezoceramic material and preparation method thereof |
CN106365621A (en) * | 2016-09-19 | 2017-02-01 | 四川行之智汇知识产权运营有限公司 | Piezoelectric nano material |
CN106587992A (en) * | 2016-12-08 | 2017-04-26 | 苏州艾博迈尔新材料有限公司 | High-performance piezoceramic material and preparation method thereof |
CN106866120A (en) * | 2015-12-11 | 2017-06-20 | 青岛祥智电子技术有限公司 | A kind of High-voltage ceramic material and preparation method thereof |
CN107304127A (en) * | 2017-07-26 | 2017-10-31 | 合肥同佑电子科技有限公司 | A kind of electronic transformer heat transmission electronic ceramics substrate and preparation method thereof |
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2017
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CN1030402A (en) * | 1987-07-06 | 1989-01-18 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Silicon nitride/boron nitride composite and manufacture method thereof |
CN102093067A (en) * | 2010-12-14 | 2011-06-15 | 江苏联能电子技术有限公司 | Nano Al2O3 crystal whisker-toughened ceramic material with high piezoelectric property and preparation method thereof |
JP2013128006A (en) * | 2011-12-16 | 2013-06-27 | Ngk Insulators Ltd | Method for manufacturing piezoelectric/electrostrictive material film |
CN105254287A (en) * | 2015-09-29 | 2016-01-20 | 苏州宽温电子科技有限公司 | Nano piezoceramic material and preparation method thereof |
CN105272327A (en) * | 2015-09-29 | 2016-01-27 | 苏州宽温电子科技有限公司 | Whisker reinforced piezoceramic material and preparation method thereof |
CN106866120A (en) * | 2015-12-11 | 2017-06-20 | 青岛祥智电子技术有限公司 | A kind of High-voltage ceramic material and preparation method thereof |
CN106365621A (en) * | 2016-09-19 | 2017-02-01 | 四川行之智汇知识产权运营有限公司 | Piezoelectric nano material |
CN106587992A (en) * | 2016-12-08 | 2017-04-26 | 苏州艾博迈尔新材料有限公司 | High-performance piezoceramic material and preparation method thereof |
CN107304127A (en) * | 2017-07-26 | 2017-10-31 | 合肥同佑电子科技有限公司 | A kind of electronic transformer heat transmission electronic ceramics substrate and preparation method thereof |
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