CN108727055A - A kind of PTC ceramic honey combs heating element and preparation method thereof - Google Patents

A kind of PTC ceramic honey combs heating element and preparation method thereof Download PDF

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Publication number
CN108727055A
CN108727055A CN201810683034.3A CN201810683034A CN108727055A CN 108727055 A CN108727055 A CN 108727055A CN 201810683034 A CN201810683034 A CN 201810683034A CN 108727055 A CN108727055 A CN 108727055A
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ceramic honey
ptc ceramic
heating element
honey combs
ptc
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邱传贡
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FENGWO ELECTRONIC PRODUCTS Co Ltd NANHAI FOSHAN
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FENGWO ELECTRONIC PRODUCTS Co Ltd NANHAI FOSHAN
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Abstract

The invention discloses a kind of PTC ceramic honey combs heating elements and preparation method thereof.The PTC ceramic honey combs heating element matches following raw material by molar ratio and is made：Ba0.73Pb0.24Ca0.03TiO1.0186%-95%, Nb2O50.03%-0.08%, Y2O30.01%-0.05%, SiO20.03%-0.08%, Al2O30.02%-0.09%, Li2CO30.1%-0.2%, MnO23%-9%, Mg2(CO3)30.1-0.5%, SiN 0.02%-0.05%.The PTC ceramic honey comb heating elements of the present invention have the advantages that interior stress balance, do not crack easily in production process, be broken, do not burst apart, be broken easily during use, have captured the technical disadvantages such as easy to crack, dilapidated walls, unfilled corner in existing production technology.

Description

A kind of PTC ceramic honey combs heating element and preparation method thereof
Technical field
The present invention relates to a kind of ceramic electric heating fields, and in particular to a kind of PTC ceramic honey combs heating element and its preparation side Method.
Background technology
Due to PTC ceramics heating element, having compared to traditional heating wire has energy saving, efficient, safe, electricity when not used Press four clear superiorities of influence of fluctuations, therefore nearly ten years its constantly expanded in substituted metal heating wire heating art, using number Amount is doubled and redoubled every year, the PTC ceramics heating element used now, is that it is (conductive simultaneous with two panels metal electrode up and down is clipped in Heat conduction), package insulating layer after be fixed on again on heat accumulation plate or radiator, the heat for sending out PTC ceramics heating element after energization Conduction blazes abroad on heat accumulation plate or radiator, achievees the effect that heating.
The cellular heating elements of PTC are with wind regime directly by the heat that PTC honeycomb elements are sent out after energization, by its own Through-hole blaze abroad by convection, it is simple in structure, it is easy to install and use, compared in identical radiating condition more than The advantages that ptc heater power of structure composition is big, small.
But if the cellular heating element inner via hole sizes of PTC are uneven, sintering process fast heating and soon cooled down Cheng Zhong, since thermal stress is uneven, the problems such as easily causing cracking, dilapidated walls, unfilled corner；Using process, due to chilling and anxious heat, It is also easy to produce phenomena such as bursting apart, being broken.
Invention content
In view of the above shortcomings of the prior art, technical problem solved by the invention is the provision of a kind of PTC honeycombs pottery Porcelain heating element, the PTC ceramic honey combs heating element can refine PTC ceramics sintering as a result of good material combination When the crystal grain that is formed, achieve the effect that shorten crystal boundary away to greatly enhance ceramic honey comb internal stress, and boundary barrier potential being made to reduce Buffering, achievees the effect that interior stress balance；And PTC ceramics sintering temperature is reduced, the generation of slow crystal grain, both may be used when promoting to be sintered Reduce PTC honeycombs in sintering since heating-cooling rate is fast, cracking phenomena when due to internal stress unevenness also helps when in use It bursts apart since chilling, anxious heat are reduced, fragmentation generates.
Technical problem solved by the invention also resides in its preparation side for providing a kind of PTC ceramic honey combs heating element Method, the technical solution can solve the technical problems such as cracking, dilapidated walls, unfilled corner in production technology.
Specific technical solution is as follows：
A kind of PTC ceramic honey combs heating element matches following raw material by mole molar ratio and is made：
Ba0.73 Pb0.24 Ca0.03 TiO1.0190%-96%, Nb2O50.03%-0.08%, Y2O3 0.01- 0.05%%, SiO20.03%-0.08%, Al2O30.02%-0.09%,
Li2CO30.1%-0.2%, MnO23%-9%, Mg2(CO3)30.1-0.5%, SiN 0.02%-0.05%.
In wherein some embodiments, the PTC ceramic honey combs heating element is made of the following raw material of mol ratio： Ba0.73 Pb0.24 Ca0.03 TiO1.0192%-94%, Nb2O50.04%-0.07%, Y2O30.01-0.03%%, SiO2 0.04%-0.07%, Al2O30.02%-0.05%, Li2CO30.1%-0.2%, MnO25%-8%, Mg2(CO3)3 0.1- 0.4%, SiN 0.02%-0.03%.
In wherein some embodiments, the PTC ceramic honey combs heating element is made of the following raw material of mol ratio： Ba0.73 Pb0.24 Ca0.03 TiO1.0193%-94%, Nb2O50.04%-0.06%, Y2O30.01-0.03%%, SiO2 0.04%-0.06%, Al2O30.02%-0.04%, Li2CO30.1%-0.2%, MnO25%-7%, Mg2(CO3)3 0.1- 0.4%, SiN 0.02%-0.03%.
Above-mentioned Ba0.73 Pb0.24 Ca0.03TiO molar ratios 1.01 are prepared using following technique：By 0.73：0.24：0.03： 21.01 molar ratio matches BaCO3、Pb2O3、CaCO3And TiO2, then it is ground and is uniformly mixed, then by BaCO3、 Pb2O3、CaCO3And TiO2Mixed material be put into corundum crucible and keep the temperature 120 minutes at 1100 DEG C~1150 DEG C, obtain BaPbCaTiO (lead barium titanate).
The present invention also provides the preparation method of above-mentioned PCT ceramic honey combs heating element, specific technical solution is as follows：
A kind of preparation method of above-mentioned PCT ceramic honey comb heating elements, includes the following steps：
(1) example is equipped with Ba in molar ratio0.73Pb0.24Ca0.03TiO1.01、Nb2O5、Y2O3、SiO2、Al2O3、Li2CO3、MnO2、 Mg2(CO3)3And SiN, obtain mixed material；
(2) mixed material obtained step (1) is added water and zirconium ball, wet Ball-stirring mill 140-160 minutes, allows each raw material It is sufficiently mixed uniformly, obtains slurry；
(3) by the slurry after wet Ball-stirring mill, with vacuum filter-press dehydration；
(4) dewatered material is contained into Xia Portland, is put into pre-burning in stove；
(5) material after pre-burning is added water and zirconium ball, wet Ball-stirring mill 190-210 minutes, then with vacuum filter-press dehydration；
(6) the pug addition vacuum after vacuum dehydration is picked and carries out picking mud in mud machine；
(7) it vacuum is picked to the material after mud puts in vacuum filter and be filtered；
(8) the specification type for pressing production requirement, corresponding honeycomb die is installed on extruder, and material mud is put tube extruding machine In, squeeze out the PTC honeycomb blanks of needs；
(9) the PTC honeycombs blank of extrusion forming is sintered by bent work in sintering condition；
(10) the PTC ceramic honey combs of sintering out, it is 0.03-0.05mm conductive silvers to stamp each thickness with silk-screen on its both sides Slurry, then with 570 DEG C of -590 DEG C of burning infiltrations, obtains the PTC ceramic honey combs heating element material.
Preferably, in the preparation method step (2) and (5) water conductive resistance >=50M Ω.
Preferably, mixed material in the preparation method step (2) and (5), water, zirconium ball weight ratio be respectively 1: 1.5:2 and 1：2：2.5.
Preferably, calcined temperature is 1000 DEG C -1200 DEG C in the preparation method step (4), soaking time 110- 130 minutes.
Preferably, suction is 0.3-0.5MPa when picking mud in the preparation method step (6), and it is 3- to pick the mud time 5 hours.
Preferably, suction is 0.6-0.7MPa in the preparation method step (7), and filtering times are 3-5 times, mistake Strainer mesh number is 200 mesh.
Compared with the prior art, the present invention program includes at least following advantageous effect：
The PTC nests ceramic heating element introduces Mg as a result of good material combination and dosage2(CO3)3, Neng Gouxi The crystal grain that is formed when changing PTC ceramics sintering, achieve the effect that shorten crystal boundary away from, to greatly enhance ceramic honey comb internal stress, and So that boundary barrier potential is reduced buffering, achievees the effect that interior stress balance；SiN is introduced, PTC ceramics sintering temperature can be reduced, promoted The generation of slow crystal grain when sintering can both reduce PTC honeycombs in sintering since heating-cooling rate is fast, due to internal stress unevenness When cracking phenomena, also help burst apart when in use since chilling, anxious heat are reduced, fragmentation generates.
Description of the drawings
Fig. 1 is the sintering curre figure of the embodiment of the present invention and comparative example.
Specific implementation mode
To facilitate the understanding of the present invention, below in conjunction with specific embodiment, the present invention will be described in more detail.But The present invention can realize in many different forms, however it is not limited to embodiment described herein.On the contrary, providing these realities The purpose for applying example is to make the disclosure of the present invention more thorough and comprehensive.
Embodiment 1
The preparation one of PTC ceramic honey comb heating elements
PTC ceramic honey comb heating elements are prepared in accordance with the following steps：
(1) each component, Ba are weighed by following molar ratio0.73 Pb0.24 Ca0.03 TiO1.01：93.54g,Nb2O5：0.05g, Y2O3：0.01g,SiO2：0.05g,Al2O3：0.05g,Li2CO3：0.15g,MnO2：6g,Mg2(CO3)3：0.1g,SiN：0.05g, Obtain mixed material；
(2) above-mentioned Ba0.73 Pb0.24 Ca0.03 TiO1.01, prepared using following technique：By 0.73：0.24：0.03： 21.01 molar ratio matches BaCO3、Pb2O3、CaCO3And TiO2, wet Ball-stirring mill is then carried out to it and is uniformly mixed, then will BaCO3、Pb2O3、CaCO3And TiO2Mixed material be put into corundum crucible inside holding 120 minutes, temperature be 1120 DEG C, obtain BaPb CaTiO (lead barium titanate).
(3) water and zirconium ball are added in said mixture material, weight ratio is mixed material, water, zirconium ball equal to 1: 1.5:2, it makes the abundant mix grinding of each raw material uniform, then grinds 150 minutes.
(4) by the slurry after wet Ball-stirring mill, with vacuum filter-press dehydration；
(5) dewatered material is contained into Xia Portland, is put into pre-burning in stove, calcined temperature is 1100 DEG C, and soaking time is 120 points Clock；
(6) by the material after pre-burning by material：Water：Zirconium ball=1:2:2.5 proportions, and wet-milling 200 minutes, then with vacuum pressure Filter dehydration.
(7) the pug addition vacuum after vacuum dehydration being picked and carries out picking mud in mud machine, suction is 0.4MPa when picking mud, It is 4 hours to pick the mud time；
(8) it vacuum is picked to the material after mud puts in vacuum filter and be filtered, suction 0.6MPa, filtering times are 4 times, filter screen mesh number is 200 mesh.
(9) the specification type for pressing production requirement, corresponding honeycomb die is installed on extruder, and material mud is put tube extruding machine In, squeeze out the PTC honeycomb blanks of needs；
(10) the PTC honeycombs blank of extrusion forming is sintered by bent work in sintering condition；
The PTC ceramic honey combs of sintering out, it is 0.05mm conductive silver pastes to stamp each thickness with silk-screen on its both sides, is then used 580 DEG C of burning infiltrations are to get to the PTC ceramic honey combs heating element.
Test result such as table 1.
Embodiment 2
The preparation two of PTC ceramic honey comb heating elements
PTC ceramic honey comb heating elements are prepared in accordance with the following steps：
(1) each component, Ba are weighed by following molar ratio0.73 Pb0.24 Ca0.03 TiO1.01：90.27,Nb2O5：0.03, Y2O3：0.03,SiO2：0.03,Al2O3：0.02,Li2CO3：0.10,MnO2：9,Mg2(CO3)3：0.5,SiN：0.02, it is mixed Material；
(2) above-mentioned Ba0.73 Pb0.24 Ca0.03 TiO1.01, prepared using following technique：By 0.73：0.24：0.03：1.01 Molar ratio match BaCO3、Pb2O3、CaCO3And TiO2, wet Ball-stirring mill is then carried out to it and is uniformly mixed, then by BaCO3、 Pb2O3、CaCO3And TiO2Mixed material be put into corundum crucible inside holding 120 minutes, temperature be 1120 DEG C, obtain Ba0PbCaTiO (lead barium titanate)
(3) water and zirconium ball are added in said mixture material, weight ratio is mixed material, water, zirconium ball equal to 1: 1.5:2, it makes the abundant mix grinding of each raw material uniform, then grinds 140 minutes.
(4) by the slurry after wet Ball-stirring mill, with vacuum filter-press dehydration；
(5) dewatered material is contained into Xia Portland, is put into pre-burning in stove, calcined temperature is 1000 DEG C, and soaking time is 110 points Clock；
(6) by the material after pre-burning by material：Water：Zirconium ball=1:2:2.5 proportions, and wet-milling 190 minutes, then with vacuum pressure Filter dehydration.
(7) the pug addition vacuum after vacuum dehydration being picked and carries out picking mud in mud machine, suction is 0.3MPa when picking mud, It is 4 hours to pick the mud time；
(8) it vacuum is picked to the material after mud puts in vacuum filter and be filtered, suction 0.6MPa, filtering times are 3 times, filter screen mesh number is 200 mesh.
(9) the specification type for pressing production requirement, corresponding honeycomb die is installed on extruder, and material mud is put tube extruding machine In, squeeze out the PTC honeycomb blanks of needs；
(10) the PTC honeycombs blank of extrusion forming is sintered by bent work in sintering condition；
The PTC ceramic honey combs of sintering out, it is 0.05mm conductive silver pastes to stamp each thickness with silk-screen on its both sides, is then used 580 DEG C of burning infiltrations are to get to the PTC ceramic honey combs heating element.
Test result such as table 1.
Embodiment 3
The preparation three of PTC ceramic honey comb heating elements
PTC ceramic honey comb heating elements are prepared in accordance with the following steps：
(1) each component, Ba are weighed by following mole0.73 Pb0.24 Ca0.03 TiO1.01：92.16,Nb2O5：0.08,Y2O3： 0.05、SiO2：0.08,Al2O3：0.09,Li2CO3：0.20,MnO2：7,Mg2(CO3)3：0.3,SiN：0.04, obtain mixture Material；
(2) above-mentioned Ba0.73 Pb0.24 Ca0.03 TiO1.01, prepared using following technique：By 0.73：0.24：0.03：1.01 Molar ratio match BaCO3、Pb2O3、CaCO3And TiO2, wet Ball-stirring mill is then carried out to it and is uniformly mixed, then by BaCO3、 Pb2O3、CaCO3And TiO2Mixed material be put into corundum crucible inside holding 120 minutes, temperature be 1120 DEG C, obtain BaPbCaTiO (lead barium titanate).
(3) water and zirconium ball are added in said mixture material, weight ratio is mixed material, water, zirconium ball equal to 1: 1.5:2, it makes the abundant mix grinding of each raw material uniform, then grinds 160 minutes.
(4) by the slurry after wet Ball-stirring mill, with vacuum filter-press dehydration；
(5) dewatered material is contained into Xia Portland, is put into pre-burning in stove, calcined temperature is 1200 DEG C, and soaking time is 120 points Clock；
(6) by the material after pre-burning by material：Water：Zirconium ball=1:2:2.5 proportions, and wet-milling 210 minutes, then with vacuum pressure Filter dehydration.
(7) the pug addition vacuum after vacuum dehydration being picked and carries out picking mud in mud machine, suction is 0.5MPa when picking mud, It is 4 hours to pick the mud time；
(8) it vacuum is picked to the material after mud puts in vacuum filter and be filtered, suction 0.7MPa, filtering times are 3 times, filter screen mesh number is 200 mesh.
(9) the specification type for pressing production requirement, corresponding honeycomb die is installed on extruder, and material mud is put tube extruding machine In, squeeze out the PTC honeycomb blanks of needs；
(10) the PTC honeycombs blank of extrusion forming is sintered by bent work in sintering condition；
The PTC ceramic honey combs of sintering out, it is 0.05mm conductive silver pastes to stamp each thickness with silk-screen on its both sides, is then used 580 DEG C of burning infiltrations are to get to the PTC ceramic honey combs heating element.
Test result such as table 1.
Comparative example
PTC ceramic honey comb heating elements are prepared in accordance with the following steps：
(1) each component, Ba are weighed by following molar ratio0.73 Pb0.24 Ca0.03 TiO1.01：93.69g,Nb2O5：0.05, Y2O3：0.01,SiO2：0.05,Al2O3：0.05,Li2CO3：0.15,MnO2：6 obtain mixed material；
(2) above-mentioned Ba0.73 Pb0.24 Ca0.03 TiO1.01, prepared using following technique：By 0.73：0.24：0.03：1.01 Molar ratio match BaCO3、Pb2O3、CaCO3And TiO2, wet Ball-stirring mill is then carried out to it and is uniformly mixed, then by BaCO3、 Pb2O3、CaCO3And TiO2Mixed material be put into corundum crucible inside holding 120 minutes, temperature be 1120 DEG C, obtain BaPb Ca TiO (lead barium titanate)
(3) water and zirconium ball are added in said mixture material, weight ratio is mixed material, water, zirconium ball equal to 1: 1.5:2, it makes the abundant mix grinding of each raw material uniform, then grinds 150 minutes.
(4) by the slurry after wet Ball-stirring mill, with vacuum filter-press dehydration；
(5) dewatered material is contained into Xia Portland, is put into pre-burning in stove, calcined temperature is 1100 DEG C, and soaking time is 120 points Clock；
(6) by the material after pre-burning by material：Water：Zirconium ball=1:2:2.5 proportions, and wet-milling 200 minutes, then with vacuum pressure Filter dehydration.
(7) the pug addition vacuum after vacuum dehydration being picked and carries out picking mud in mud machine, suction is 0.4MPa when picking mud, It is 4 hours to pick the mud time；
(8) it vacuum is picked to the material after mud puts in vacuum filter and be filtered, suction 0.6MPa, filtering times are 4 times, filter screen mesh number is 200 mesh.
(9) the specification type for pressing production requirement, corresponding honeycomb die is installed on extruder, and material mud is put tube extruding machine In, squeeze out the PTC honeycomb blanks of needs；
(10) the PTC honeycombs blank of extrusion forming is sintered by bent work in sintering condition；
The PTC ceramic honey combs of sintering out, it is 0.05mm conductive silver pastes to stamp each thickness with silk-screen on its both sides, is then used 580 DEG C of burning infiltrations are to get to the PTC ceramic honey combs heating element.
Test result such as table 1.
Table 1
Can be seen that from the qualification rate test data in table 1 with multimeter ohms range sorting room temperature resistance is 30-80 Ω When PTC ceramic honey combs are certified products, before being not introduced into Mg2 (CO3) 3 and SiN in the feed, the conjunction of PTC ceramic honey comb heating elements Lattice rate is 60%, and after introducing Mg2 (CO3) 3 and SiN, qualification rate is obviously improved, and has reached 85%~86%, and appearance is without disconnected Split, burst apart, the qualification rate of unfilled corner is even more to reach 95%~96%, greatly reduce cracking in production technology, dilapidated walls, unfilled corner and ask Topic.
Every technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned The all possible combination of each technical characteristic in embodiment is all described, as long as however, the combination of these technical characteristics not There are contradictions, are all considered to be the range of this specification record.
Embodiment described above only describes the several embodiments of the present invention, the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (10)

1. a kind of PTC ceramic honey combs heating element, which is characterized in that the PTC ceramic honey combs heating element is by following molar ratio Raw material is made：
2. PTC ceramic honey combs heating element according to claim 1, which is characterized in that the PTC ceramic honey combs heating unit Part is made of the following raw material of mol ratio：
3. PTC ceramic honey combs heating element according to claim 2, which is characterized in that the PTC ceramic honey combs heating unit Part is made of the following raw material of mol ratio：
4. according to claim 1-3 any one of them PTC ceramic honey comb heating elements, which is characterized in that described Ba0.73Pb0.24Ca0.03TiO1.01It is prepared using following technique：By 0.73：0.24：0.03：1.01 molar ratio matches BaCO3、 Pb2O3、CaCO3And TiO2, then it is ground and is uniformly mixed, then by BaCO3、Pb2O3、CaCO3And TiO2Mixture Material is put into corundum crucible and keeps the temperature 120 minutes at 1100 DEG C~1150 DEG C, obtains BaPb CaTiO (lead barium titanate).
5. a kind of preparation method of PTC ceramic honey combs heating element as claimed in any one of claims 1-3, it is characterised in that Include the following steps：
(1) it is equipped with Ba in proportion0.73Pb0.24Ca0.03TiO1.01、Nb2O5、Y2O3、SiO2、Al2O3、Li2CO3、MnO2、Mg2(CO3)3 And SiN, obtain mixed material；
(2) water and zirconium ball is added in the mixed material for obtaining step (1), wet Ball-stirring mill 140-160 minutes, makes each raw material abundant It is uniformly mixed, obtains slurry；
(3) by the slurry after wet Ball-stirring mill, with vacuum filter-press dehydration；
(4) dewatered material is contained into Xia Portland, is put into pre-burning in stove；
(5) water and zirconium ball is added in the material after pre-burning, wet Ball-stirring mill 190-210 minutes, each raw material is allowed to be sufficiently mixed uniformly, then With vacuum filter-press dehydration；
(6) the pug addition vacuum after vacuum dehydration is picked and carries out picking mud in mud machine；
(7) it vacuum is picked to the material after mud puts in vacuum filter and be filtered；
(8) the specification type for pressing production requirement, corresponding honeycomb die is installed on extruder, and material mud is put in tube extruding machine, Squeeze out the PTC honeycomb blanks needed；
(9) the PTC honeycombs blank of extrusion forming is sintered by bent work in sintering condition；
(10) the PTC ceramic honey combs of sintering out, it is 0.03-0.05mm conductive silver pastes to stamp each thickness with silk-screen on its both sides, so Afterwards with 570 DEG C of -590 DEG C of burning infiltrations, the PTC ceramic honey combs heating element material is obtained.
6. the preparation method of PTC ceramic honey combs heating element as claimed in claim 5, which is characterized in that the preparation side The conductive resistance of water >=50M Ω in method step (2) and (5).
7. the preparation method of PTC ceramic honey combs heating element as claimed in claim 5, which is characterized in that the preparation side Mixed material in method step (2) and (5), water, zirconium ball weight ratio be respectively 1:1.5:2 and 1：2：2.5.
8. the preparation method of PTC ceramic honey combs heating element as claimed in claim 5, which is characterized in that the preparation side Calcined temperature is 1000 DEG C -1200 DEG C in method step (4), and soaking time is 110-130 minutes.
9. the preparation method of PTC ceramic honey combs heating element as claimed in claim 5, which is characterized in that the preparation side Suction is 0.3-0.5MPa when picking mud in method step (6), and it is 3-5 hours to pick the mud time.
10. the preparation method of PTC ceramic honey combs heating element as claimed in claim 5, which is characterized in that the preparation side Suction is 0.6-0.7MPa in method step (7), and filtering times are 3-5 times, and filter screen mesh number is 200 mesh.
CN201810683034.3A 2018-06-27 2018-06-27 A kind of PTC ceramic honey combs heating element and preparation method thereof Pending CN108727055A (en)

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