CN107867852A - Low temperature co-fired PTC ceramic materials constituent - Google Patents

Low temperature co-fired PTC ceramic materials constituent Download PDF

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CN107867852A
CN107867852A CN201610856032.0A CN201610856032A CN107867852A CN 107867852 A CN107867852 A CN 107867852A CN 201610856032 A CN201610856032 A CN 201610856032A CN 107867852 A CN107867852 A CN 107867852A
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ptc
pbo
ceramic material
ceramic
low temperature
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盖浩然
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Qingdao Dong Hao Software Technology Co Ltd
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Qingdao Dong Hao Software Technology Co Ltd
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Abstract

The present invention relates to a kind of new PTC-ceramic material constituent, is a kind of low temperature co-fired PTC-ceramic material constituent specifically.The constituent, including ceramic phase and glass phase, it is characterised in that：The ceramic phase is conventional PTC-ceramic material, and the glass is mutually PbO BN materials, and the content of the PbO BN materials is 1 10wt%, and the content of PTC-ceramic material is 90 99wt%.This product is mutually made to reduce PTC-ceramic material sintering temperature using PbO BN glass, while has high-performance ptc characteristicses, and use range is wide.

Description

Low temperature co-fired PTC-ceramic material constituent
Technical field
The present invention relates to a kind of new PTC-ceramic material constituent, is a kind of low temperature co-fired PTC-ceramic material specifically Expect constituent.
Background technology
In recent years, semiconductor technology rapid development drive under, electronic component constantly to miniaturization, it is integrated and high Frequencyization direction is developed.With the fast development of SMT technologies, the small-sized of electronic equipment and electronic component has been greatly facilitated Change, miniaturization, integrated and chip type, and developing preparation, there is the chip type of sandwich construction, the PTC-element of miniaturization to turn into state Inside and outside study hotspot and emphasis.In order to realize the chip type of sandwich construction PTC-element, miniaturization, used ptc material must Must possess in the low-temperature sintering condition good PTC effects of big holding and higher proof voltage, relatively low resistivity；To ensure its energy It is applied in microcircuit and other more extensive scopes, this make it that how research prepares and can be sintered at low temperature And the ceramic composition of high-performance ptc characteristicses is kept to turn into the key of technology.It is the core skill for realizing that ptc material is low temperature co-fired Art, it is the basis for preparing sandwich construction PTC-element.
The optimum technical scheme of PTC-element for preparing sandwich construction is to use for reference MLCC low temperature co-firing technologies, although so The PTC-element of low temperature co-fired sandwich construction has extremely strong inheritance in structure and manufacture craft with MLCC, but due to BaTiO 3 be that high posistor material sintering temperature, exogenous impurity or the second phase usually influence semiconducting degree, or even is led The inherent characteristics such as its exhausted rafter are caused, so find the glass phase ten for reducing its sintering temperature and the Ohm contact electrode that can be burnt altogether therewith Point difficulty, realizing the process line of only petrochemical industry, to become difficulty larger.It is low to be placed on preparation high-performance low-resistivity for main research at present Above the porcelain of sintering temperature；Its key technology is studied for low temperature co-fired PTC-ceramic constituent.
Such as a kind of base laminated slice type PTC heat sensitive resistors of BaTiO 3 disclosed in Chinese invention patent ZL03128233.4 Preparation technology, include successively：1. chip PTC green compact are prepared using film rolling forming process；2. electrode in sputtering；3. burn altogether；4. shape Into termination electrode.The technique has advantages below：Chip PTC green compact are prepared using rolling formation method, using water as solvent, because And environmental pollution is small, labor intensity is low, and easily operated and cost is cheap.Blank made from rolling formation has necessarily uniform Degree, consistency and finish, and the pliability of film base is preferable, has good processing performance.Using hot pressing sintering method, sintering During be easily formed good Ohmic contact.Using first burning base substrate and interior electrode altogether in reducing atmosphere, then relatively low At a temperature of make the sintering processing of porcelain body grain boundary oxidation as oxidation processes, efficiently solve the problem of oxidation of metal electrode, and shape Into good PTC effects.Can be flexible come regulating element characteristic, method by changing the number of plies of lamination raw cook and the thickness of raw cook It is and easy.
In terms of the technology announced a few days ago, so far there are no mutually makees to reduce PTC-ceramic material sintering temperature using PbO-BN glass Degree, while there is the report of the PTC-ceramic material of high-performance ptc characteristicses.Therefore, offer one kind is provided and uses PbO-BN glass phases Make to reduce PTC-ceramic material sintering temperature, while there is the low temperature co-fired PTC-ceramic material constituent of high-performance ptc characteristicses.
The content of the invention
Mutually make reduction PTC-ceramic material sintering temperature using PbO-BN glass it is an object of the invention to provide one kind, simultaneously Low temperature co-fired PTC-ceramic material constituent with high-performance ptc characteristicses.
The present invention basic conception be：A kind of low temperature co-fired PTC-ceramic material constituent, the constituent is by ceramic phase and glass Glass phase composition.Its ceramic phase is that common BaTiO 3 is PTC-ceramic material (hereinafter referred to as PTC-ceramic material), and glass is mutually PbO-BN materials.The content of PTC-ceramic material is 90-99wt%, and the content of PbO-BN materials is 1-10wt%.Optimal proportion For：The total content of PTC-ceramic material is 94-97wt%, and PbO-BN glass contains 3-6%wt；In PbO-BN materials：PbO and BN Mol ratio be 1.5-2.PTC-ceramic material needs artificial synthesized in advance；PbO-BN materials are claimed by PbO and BN mol ratio in advance Amount, then ball milling mixing is standby；Two kinds of material particle size scopes are between 0.5-1.5 μm.
The invention provides it is a kind of can with nickel slurry at 1200 DEG C and its it is following low temperature co-fired and make PTC-ceramic material Material, can apply to the PTC-element for possessing sandwich construction of various uses.It is an object of the invention to overcome the above-mentioned of prior art Deficiency, prepares and disclosure satisfy that PTC-element requirement, can, low temperature co-fired PTC glass that resistivity lower pottery low temperature co-fired with nickel slurry Ceramic material constituent, especially provide a kind of PTC-element constituent suitable for sandwich construction；The PTC constituents can less than Sintering prepares excellent PTC-element under the conditions of 150-200 DEG C of nominal sintering temperatures, can be achieved low temperature co-fired with Ni electrodes.Energy Meet the manufacture of the PTC themistor of all kinds of sandwich constructions, starched using ceramic slurry prepared by the PTC constituents and interior nickel The PTC that material produces all kinds of sandwich constructions of function admirable by being cast, printing the technique such as folded, cutting and control climate sintering together Thermal resistor.BN is a kind of very effective sintering mineralizer, and liquid phase can be produced at 1100 DEG C, promotes ceramic post sintering, So as to reduce sintering temperature.PbO is also a kind of very effective sintering mineralizer, and also can produce liquid phase at 890 DEG C adds Add, independent BN or PbO are unfavorable for reducing ρ 25 and keep PTC effects not deteriorate；Because Pb and BN is to the matrix PTC materials of BaTiO 3 Performance all have a great impact, every electrical property of ptc material can be had a strong impact on after addition.The present invention is found through experiments that Addition BN makees to add PbO while sintering aid, not only can further reduce sintering temperature but also can obviously improve because of BN and BaTiO 3 It is the compatibility of ceramics, finds to ensure that the certain stoichiometric proportions of PbO and BN not only improve reduction and burn till temperature through further experiment Degree is again not clear to influence room temperature resistivity and PTC effects, can reduce about 150-200 DEG C ceramic of sintering temperature of the systems of BaTiO 3.The party Ptc material function admirable prepared by method, PTC effects are without obvious deterioration.
Specifically, low temperature co-fired PTC-ceramic material constituent of the invention, including ceramic phase and glass phase, its feature It is：The ceramic phase is conventional PTC-ceramic material, and the glass is mutually PbO-BN materials, the content of the PbO-BN materials For 1-10wt%, the content of PTC-ceramic material is 90-99wt%.Optimal proportion is：PbO-BN materials contain 3-6%wt, PTC The content of ceramic material is 94-97wt%.
In the PbO-BN materials：PbO and BN mol ratio is 1.5-2, and PTC-ceramic material is artificial synthesized in advance. The PbO-BN materials press PbO and BN molar ratio weighing in advance, and then ball milling mixing is standby raw materials used after ball milling, two kinds Material particle size scope is between 0.5 to 1.5 μm.Using above-mentioned technical proposal, the prominent technological progress of the present invention is：1、 It is PTC thermistor material energy this compatible feature very well using PbO-BN and BaTiO 3, after this material pre-burning is synthesized Conventional BaTiO 3 is that the mixing of PTC thermistor material can be with low temperature co-fired PTC-ceramic porcelain with regard to that can prepare.2nd, with PbO- BN is PTC thermistor material as function ceramics phase using conventional BaTiO 3, thus as the glass phase for reducing sintering temperature The PTC glass ceramic materials of gained both can be low temperature co-fired with nickel slurry under 1200 DEG C and its following temperature, also has foot Enough excellent PTC effects.3rd, by described low temperature co-fired PTC glass ceramic materials constituent, after ball milling, particle chi Very little scope is between 0.5 to 5.0 μm.Relatively thin casting films can be formed, and can ensures what can be starched during porcelain body sintering shrinkage with nickel Sintering shrinkage matches, and can cause slice, thin piece deformation or even ftracture, can prepare function admirable has the PTC-element of sandwich construction.
Compared with the aforementioned existing similar products, low temperature co-fired PTC-ceramic material constituent of the invention uses PbO-BN glass Glass is mutually made to reduce PTC-ceramic material sintering temperature, while has high-performance ptc characteristicses, and use range is wide.
Present disclosure is further described with the following Examples, but present disclosure is not limited only to implement Involved content in example.Embodiment applies a certain particular requirement with overtemperature protection：Room temperature resistance≤100 Ω, temperature coefficient ＞ 18%/DEG C, for Curie temperature at 120 DEG C, proof voltage ＞ 30V make specific implementation explanation.
Embodiment
Embodiment 1：
A kind of low temperature co-fired PTC-ceramic material constituent, the constituent is by ceramic phase and glass phase composition.Its ceramic phase is Common PTC-ceramic material, glass are mutually PbO-BN based materials.The mol ratio of PbO-BN materials is 1.5.Now PbO and BN Percentage by weight is：PbO: BN=93: 7 (wt%)
PTC-ceramic material need to be pre-synthesis, and its technological process synthesized is：
BaCO3、TiO2、Y2O3、SrCO3、CaCO3、SiO2With Mn (NO3)2, according to the change of following common PTC-ceramic materials Learn equation (1)：
Ba0.85Ca0.15Ti1.01O3+ 0.25mol%Y2O3+ 2.4mol%SiO2+ 0.08mol%Mn (NO3)2(1)
Mix-ball milling-drying-pre-burning synthesis is carried out, the temperature of pre-burning synthesis is with 1100 DEG C to 1200 DEG C Preferably.
PbO-BN materials need to be pre-mixed, and its technological process mixed is：
PbO and BN is 1.5 according to mol ratio.Equivalent PbO and BN percentage by weight is：PbO: BN=93: 7 (wt%'s) Ratio is weighed, and standby PbO-BN materials are obtained by processes such as mix-ball milling-dryings.
Then requirement PTC-ceramic material and PbO-BN materials mixed by formula dispensing：Weighing-ball milling-drying, is obtained Obtain low temperature co-fired PTC-ceramic material composition powder.The particle size of porcelain is after ball milling：1.0-1.5μm.
The powder is configured to casting slurry and carries out tape casting operation using casting machine, ceramic diaphragm after curtain coating and nickel slurry are printed Folded five layers of formation bar block, then designs cut lengths and direction by finished size 1.0 × 1.0 × 05, is cut into sandwich construction Ceramic green.Above-mentioned green compact are put into sintering furnace and carry out freezing of a furnace, insulation is sintered for 1 hour, obtains BaTiO3 systems Semiconductive ceramic matrix, by the electron microscope observation ceramic body grain size in 2-4 μ.Potsherd is smeared into In-Ga electricity Pole.
Embodiment two
A kind of low temperature co-fired PTC-ceramic material constituent, the constituent is by ceramic phase and glass phase composition.Its ceramic phase is Common PTC-ceramic material, glass are mutually PbO-BN materials.The mol ratio of PbO-BN materials is 2.Now PbO and BN weight Percentage is：PbO: BN=95: 5 (wt%)
PTC-ceramic material need to be pre-synthesis, and its technological process synthesized is：
BaCO3, TiO2, Y2O3, SrCO3, CaCO3, SiO2 and Mn (NO3) 2, according to following common PTC-ceramic materials Chemical equation (1)：
Ba0.85Ca0.15Ti1.01O3+0.25mol%Y2O3+2.4mol%SiO2+0.08mol%Mn (NO3) 2 (1)
Mix-ball milling-drying-pre-burning synthesis is carried out, the temperature of pre-burning synthesis is with 1100 DEG C to 1200 DEG C Preferably.
PbO-BN materials need to be pre-mixed, and its technological process mixed is：
PbO and BN is 2 according to mol ratio.Equivalent PbO and BN percentage by weight is：PbO: BN=95: 5 (wt%) ratio Example is weighed, and standby PbO-BN materials are obtained by processes such as mix-ball milling-dryings.
Then requirement PTC-ceramic material and PbO-BN materials mixed by formula dispensing：Weighing-ball milling-drying, is obtained Obtain low temperature co-fired PTC-ceramic material composition powder.The particle size of porcelain is 1.0-1.5 μm after ball milling.
The powder is configured to casting slurry and carries out tape casting operation using casting machine, ceramic diaphragm after curtain coating and nickel slurry are printed Folded five layers of formation bar block, then designs cut lengths and direction by finished size 1.0 × 1.0 × 05, is cut into sandwich construction Ceramic green.Above-mentioned green compact are put into sintering furnace and carry out freezing of a furnace, insulation is sintered for 1 hour, obtains BaTiO3 systems Semiconductive ceramic matrix, by the electron microscope observation ceramic body grain size in 2-4 μ.Potsherd is smeared into In-Ga electricity Pole.
Typical embodiment described above for the present invention, but the present invention should not be limited to above-described embodiment institute public affairs The content opened.It is every not depart from the lower equivalent or modification completed of spirit disclosed in this invention, it should all fall into what the present invention protected Scope.

Claims (4)

1. a kind of low temperature co-fired PTC-ceramic material constituent, including ceramic phase and glass phase, it is characterised in that：The ceramic phase For conventional PTC-ceramic material, the glass is mutually PbO-BN materials, and the content of the PbO-BN materials is 1-10wt%, and PTC makes pottery The content of ceramic material is 90-99wt%.
2. low temperature co-fired PTC-ceramic material constituent according to claim 1, it is characterised in that the PbO-BN materials In：PbO and BN mol ratio is 1.5-2, and PTC-ceramic material is artificial synthesized in advance.
3. low temperature co-fired PTC-ceramic material constituent according to claim 1 or 2, it is characterised in that the PbO-BN materials Material presses PbO and BN molar ratio weighing in advance, and then ball milling mixing is standby.
4. low temperature co-fired PTC-ceramic material constituent according to claim 3, it is characterised in that：It is raw materials used through ball milling Afterwards, particle size range is between 0.5 to 1.5 μm.
CN201610856032.0A 2016-09-27 2016-09-27 Low temperature co-fired PTC ceramic materials constituent Pending CN107867852A (en)

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