CN116813325A - Production process of thermosensitive ceramic - Google Patents
Production process of thermosensitive ceramic Download PDFInfo
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- CN116813325A CN116813325A CN202310339079.XA CN202310339079A CN116813325A CN 116813325 A CN116813325 A CN 116813325A CN 202310339079 A CN202310339079 A CN 202310339079A CN 116813325 A CN116813325 A CN 116813325A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 150
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 57
- 238000000498 ball milling Methods 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 40
- 238000000227 grinding Methods 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000005303 weighing Methods 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005520 cutting process Methods 0.000 claims abstract description 15
- 229910052709 silver Inorganic materials 0.000 claims abstract description 15
- 239000004332 silver Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000004615 ingredient Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 230000003068 static effect Effects 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims description 14
- 239000005995 Aluminium silicate Substances 0.000 claims description 13
- 229910052582 BN Inorganic materials 0.000 claims description 13
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 13
- 235000012211 aluminium silicate Nutrition 0.000 claims description 13
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 10
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052863 mullite Inorganic materials 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 18
- 230000000052 comparative effect Effects 0.000 description 32
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- 229910052742 iron Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 206010057040 Temperature intolerance Diseases 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000008543 heat sensitivity Effects 0.000 description 2
- -1 liCl 2Al (OH) 3 nH2O Chemical compound 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 210000001161 mammalian embryo Anatomy 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910001148 Al-Li alloy Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The application relates to a production process of thermosensitive ceramic. The preparation method comprises the following preparation steps: 1): respectively standing the heat-sensitive ceramic raw materials, and sealing and preserving to obtain a standby ingredient; 2): weighing the ingredients to be used respectively, mixing to obtain a mixture, ball-milling the mixture with water, and drying to obtain a ball grinding material; 3): sieving the ball milling material, presintering to obtain presintering material; 4): mixing the mixture with water, and ball milling to obtain a second abrasive; 5): carrying out static pressure molding and sintering on the two grinding materials to obtain a ceramic core ingot; 6): cutting a ceramic core ingot into ceramic sheets, coating silver paste on the surfaces of the ceramic sheets, solidifying and cutting to obtain the heat-sensitive ceramic: in the process, the raw materials of the thermosensitive ceramic are finer through the grinding balls for two times, the raw materials are fully and uniformly mixed, and the compatibility of a raw material system is further improved through preheating treatment, so that the compactness of the prepared thermosensitive ceramic is improved, and the thermosensitive ceramic has a better thermosensitive effect.
Description
Technical Field
The application relates to the field of electronic materials, in particular to a production process of thermosensitive ceramics.
Background
The thermal ceramic is a kind of functional ceramic with resistivity obviously changing with temperature. A ceramic material having a zero power resistance that varies with temperature over an operating temperature range. The method is mainly used for manufacturing thermistors, temperature sensors, heaters, current limiting elements and the like.
With the development of technology, thermal ceramics become an essential component of daily life due to their temperature-sensitive property. In particular, NTC and PTC thermal ceramics are mainly characterized in that they realize the expected operation of the device as an on-temperature difference at the curie temperature point in a temperature control system.
The thermosensitive ceramic is prepared by mixing various oxides and sintering at high temperature in the production process, but the existing thermosensitive ceramic has low compactness, so that the thermosensitive effect of the thermosensitive ceramic is reduced.
Disclosure of Invention
In order to improve the thermosensitive effect of thermosensitive ceramics, the application provides a production process of thermosensitive ceramics.
The production process of the thermosensitive ceramic provided by the application adopts the following technical scheme:
a production process of thermosensitive ceramics comprises the following preparation steps:
1): standing the heat sensitive ceramic raw materials for 6-9h respectively, and sealing and preserving to obtain a standby ingredient;
2): weighing the ingredients to be used respectively according to the weight percentage, mixing to obtain a mixture, mixing 200-300 parts of the mixture with 380-420 parts of water, ball milling for 4-6 hours, and drying to obtain the ball grinding material;
3): sieving the ball milling material, presintering for 4-6 hours at 700-900 ℃ to obtain presintering material;
4): mixing 200-300 parts of the mixture with 380-420 parts of water according to parts by weight, and ball milling for 7-9 hours to obtain a secondary grinding material;
5): carrying out static pressure molding on the secondary grinding material to obtain a ceramic blank, and sintering the ceramic blank for 5-7h at the temperature of 1200-1300 ℃ to obtain the ceramic blank;
6): cutting the ceramic core ingot into ceramic sheets, coating silver paste on the surfaces of the ceramic sheets, curing at 780-850 ℃, and cutting to obtain the thermosensitive ceramic.
The process operation has high production efficiency, and the obtained thermosensitive ceramic has good compactness, and the thermosensitive constant of the thermosensitive ceramic is up to 3950+/-3%.
Through standing the thermal sensitive ceramic raw materials for 6-9h and then sealing, the thermal sensitive ceramic raw materials are kept in the same state, so that the subsequent processing is facilitated; after the ingredients are mixed, the mixture is ground with water to ensure that all the raw materials in the thermosensitive ceramic raw material system are fully and uniformly mixed.
The ball grinding material is presintered for 4-6 hours at 700-900 ℃, so that the heat-sensitive ceramic raw material is heated and expanded, the subsequent grinding ball is facilitated, grinding is performed again, the improvement of the fineness of the ball grinding material is facilitated, when the two grinding materials are subjected to static pressure, the two grinding materials can fully fill a die, and the ceramic core ingot with higher ceramic core ingot is obtained after sintering for 5-7 hours at 1200-1300 ℃, and the obtained heat-sensitive ceramic has better heat-sensitive effect after the ceramic core ingot is subjected to cutting, silver paste coating, 780-850 ℃ curing and other processes.
The preferable raw materials of the thermosensitive ceramic consist of the following raw materials in percentage by weight:
NiO：5-9％
Mn 3 O 4 ：46-50％
Fe 2 O 3 ：13-18％
Zn：23-27％
ZnO：1-8％。
preferably, the mixture of 2) is obtained by the following method: weighing NiO, mn3O4, fe2O3, zn and ZnO according to the weight percentage, and mixing to obtain the mixture.
Through NiO, mn 3 O 4 、Fe 2 O 3 Zn and ZnO are used as raw materials, and the obtained semiconductor ceramic core ingot has better compactness, so that the prepared thermosensitive ceramic has better thermosensitive effect.
Preferably, the standing temperature in 1) is 23-27 ℃ and the relative humidity is 27-35%.
The heat-sensitive ceramic raw material left standing can be kept in a constant state at the above humidity and temperature.
Preferably, the ball milling rate in the steps 1) and 2) is 150-200r/min.
The ball milling speed is selected to fully and uniformly mix the raw material system of the thermosensitive ceramic, so that the compactness of the thermosensitive ceramic is improved.
Preferably, the number of the sieves in 3) is 100-800 mesh.
The number range is selected, so that the raw materials of the thermosensitive ceramic can fully fill the die to form the thermosensitive ceramic with compact structure, and the thermosensitive effect of the thermosensitive ceramic is improved.
Preferably, the thickness of the ceramic sheet is 0.40-0.50mm.
Preferably, the silver paste in 5) is coated to a thickness of 50-100 μm.
The silver paste with the thickness range is selected, so that the obtained thermosensitive ceramic has better thermosensitive effect.
Preferably, the raw materials of the thermosensitive ceramic consist of the following raw materials in percentage by weight:
adsorption composite 13-15%
NiO：5-9％
Mn 3 O 4 ：36-40％
Fe 2 O 3 ：10-15％
Zn：23-27％
ZnO：1-3％。
Through NiO, mn 3 O 4 、Fe 2 O 3 Zn, znO and adsorption compound are used as raw materials, so that the obtained ceramic core ingot has compact structure and the thermosensitive effect of thermosensitive ceramic is improved.
The added adsorption compound is not only sensitive to heat, but also has insulating effect and adhesiveness, and when two abrasive materials are subjected to static pressure forming, the raw materials are tightly combined, so that the prepared ceramic core ingot has better compactness, and the heat-sensitive effect of heat-sensitive ceramic is improved.
Preferably, the adsorption compound is prepared from kaolin, liCl 2Al (OH) 3.nH2O, hexagonal boron nitride and mullite powder in a weight ratio of 3: (1.2-1.5): (1.5-1.8): (1.3-1.7).
The kaolin is clay, the crystal chemical formula of the kaolin is 2SiO2.Al2O3.2H2O, nitrogen and boron in hexagonal boron nitride also form a hexagonal net-shaped layer, and the hexagonal boron nitride are mutually overlapped to form crystals, so that the hexagonal boron nitride has good insulation property and thermal conductivity, is sensitive to heat, is mainly used as a refractory material and a semiconductor solid-phase doping source, and can improve the thermosensitive effect of thermosensitive ceramics when being added.
Mullite of formula 3A 2 lO 3 ·2SiO 2 Contains A 2 lO 3 And SiO 2 The strength of the ceramic is improved.
LiCl 2Al (OH) 3 nH2O aluminum lithium compound contains rare metal Li, and when the internal structure of the thermal ceramic is improved in the calcining process, the thermal ceramic becomes more compact, so that the thermal effect of the thermal ceramic is improved.
Therefore, the adsorption compound obtained by compounding mullite, liCl 2Al (OH) 3 nH2O, kaolin and hexagonal boron nitride has better viscosity, insulativity, thermal conductivity, strength and the like, so that the ceramic core ingot has a tighter structure, and the obtained thermosensitive ceramic has better thermal conduction effect.
In summary, the application has the following beneficial effects:
1. the raw materials of the thermosensitive ceramic are finer through the grinding balls for two times, the raw materials are fully and uniformly mixed, and the compatibility of a raw material system is further improved through preheating treatment, the compactness of the prepared thermosensitive ceramic is improved, and the thermosensitive ceramic has a better thermosensitive effect.
2. The adsorption compound obtained by compounding mullite, liCl 2Al (OH) 3 nH2O, kaolin and hexagonal boron nitride has better viscosity, insulativity, thermal conductivity, strength and the like, so that the ceramic core ingot has a tighter structure, and the obtained thermosensitive ceramic has better thermal conductivity.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
A production process of thermosensitive ceramics comprises the following steps:
1): niO, mn 3 O 4 、Fe 2 O 3 And respectively standing the Zn and ZnO thermosensitive ceramic raw materials at a constant temperature and constant humidity for 8 hours, wherein the standing temperature is 25 ℃, and the relative humidity is 30 percent, and respectively transferring the raw materials into a medicine box for sealing and preserving to obtain the ingredients for later use.
2): weighing 7.5% of NiO and 48.5% of Mn according to weight percentage 3 O 4 、16％Fe 2 O 3 Mixing 25% of Zn and 3% of ZnO to obtain a mixture; putting 250g of the mixture and 400g of deionized water into a ball mill, ball milling for 5 hours at a ball milling rate of 180r/min, and puttingAnd (5) putting the mixture into a baking oven at 50 ℃ for baking for 5 hours to obtain the ball grinding material.
3): and (3) sieving the ball milling material obtained in the step (2) through a 300-mesh sieve to obtain 300-mesh ball milling materials, heating the 300-mesh ball milling materials to 800 ℃ in a bell jar furnace, and presintering for 5 hours to obtain the presintering material.
4): weighing 250g of the pre-sintered material obtained in 3) and 400g of deionized water, putting the pre-sintered material and the 400g of deionized water into a ball mill, and performing ball milling for 8 hours at a ball milling rate of 180r/min to obtain the secondary grinding material.
5): and (3) placing the second abrasive into a die, pressing the die by adopting 20N force to perform static pressure molding on the second abrasive to obtain a ceramic blank, placing the ceramic blank into a bell jar furnace, and sintering at the temperature of 1250 ℃ for 6 hours to obtain a ceramic core ingot.
6): cutting a ceramic core ingot into ceramic sheets with the thickness of 0.45mm, coating silver paste on the surfaces of the ceramic sheets, coating the ceramic sheets with the thickness of 80 mu m, and curing for 20s at the temperature of 800 ℃ to enable the ceramic sheets and the silver layers to be tightly combined for cutting, thus obtaining the thermosensitive ceramic.
Example 2
A production process of thermosensitive ceramics comprises the following steps:
1): niO, mn 3 O 4 、Fe 2 O 3 And respectively standing the Zn and ZnO thermosensitive ceramic raw materials at a constant temperature and constant humidity for 6 hours, wherein the standing temperature is 27 ℃, the relative humidity is 27%, and respectively transferring the raw materials into a medicine box for sealing and preserving to obtain the ingredients for later use.
2): weighing 7.5% of NiO and 48.5% of Mn according to weight percentage 3 O 4 、16％Fe 2 O 3 Mixing 25% of Zn and 3% of ZnO to obtain a mixture; and (3) putting 250g of the mixture and 400g of deionized water into a ball mill, performing ball milling for 4 hours at a ball milling rate of 200r/min, and then putting into a 50 ℃ oven for drying for 4 hours to obtain the ball grinding material.
3): and (3) sieving the ball milling material obtained in the step (2) through a 100-mesh sieve to obtain 100-mesh ball milling materials, heating the 100-mesh ball milling materials to 700 ℃ in a bell jar furnace, and presintering for 4 hours to obtain the presintering material.
4): weighing 250g of the pre-sintered material obtained in 3) and 400g of deionized water, putting the pre-sintered material and the 400g of deionized water into a ball mill, and performing ball milling for 7 hours at a ball milling rate of 200r/min to obtain a secondary grinding material;
5): and (3) placing the second abrasive into a die, pressing the die by adopting 20N force to perform static pressure molding on the second abrasive to obtain a ceramic blank, placing the ceramic blank into a bell jar furnace, and sintering for 7h at the temperature of 1200 ℃ to obtain the ceramic core ingot.
6): cutting a ceramic core ingot into ceramic sheets with the thickness of 0.40mm, coating silver paste on the surfaces of the ceramic sheets, coating the ceramic sheets with the thickness of 100 mu m, and curing for 20s at the temperature of 780 ℃ to enable the ceramic sheets and the silver layers to be tightly combined for cutting, thus obtaining the thermosensitive ceramic.
Example 3
A production process of thermosensitive ceramics comprises the following steps:
1): niO, mn 3 O 4 、Fe 2 O 3 And respectively standing the Zn and ZnO thermosensitive ceramic raw materials for 9 hours at the constant temperature and humidity, wherein the standing temperature is 23 ℃, the relative humidity is 35%, and respectively transferring the raw materials into a medicine box for sealing and preserving to obtain the ingredients for later use.
2): weighing 7.5% of NiO and 48.5% of Mn according to weight percentage 3 O 4 、16％Fe 2 O 3 Mixing 25% of Zn and 3% of ZnO to obtain a mixture; and (3) putting 250g of the mixture and 400g of deionized water into a ball mill, performing ball milling for 6 hours at a ball milling rate of 150r/min, and then putting into a 50 ℃ oven for drying for 6 hours to obtain the ball grinding material.
3): and (3) sieving the ball milling material obtained in the step (2) through a 500-mesh sieve to obtain 500-mesh ball milling materials, heating the 500-mesh ball milling materials to 900 ℃ in a bell jar furnace, and presintering for 6 hours to obtain the presintering material.
4): weighing 250g of the pre-sintered material obtained in 3) and 400g of deionized water, putting the pre-sintered material and the 400g of deionized water into a ball mill, and performing ball milling for 8 hours at a ball milling rate of 180r/min to obtain the secondary grinding material.
5): and (3) placing the second abrasive into a die, pressing the die by adopting 20N force to perform static pressure molding on the second abrasive to obtain a ceramic blank, placing the ceramic blank into a bell jar furnace, and sintering for 5 hours at the temperature of 1300 ℃ to obtain a ceramic core ingot.
6): cutting a ceramic core ingot into ceramic sheets with the thickness of 0.50mm, coating silver paste on the surfaces of the ceramic sheets, coating the ceramic sheets with the thickness of 100 mu m, and curing for 20s at the temperature of 850 ℃ to enable the ceramic sheets and the silver layers to be tightly combined for cutting, thus obtaining the thermosensitive ceramic.
Example 4
Example 4 differs from example 1 in that: 5% NiO, 50% Mn 3 O 4 、13％Fe 2 O 3 、27％Zn、5％ZnO。
Example 5
Example 5 differs from example 1 in that: 9% NiO, 46% Mn 3 O 4 、18％Fe 2 O 3 、23％Zn、4％ZnO。
Example 6
Example 6 differs from example 1 in that the raw material composition of the thermal ceramics is different, specifically as shown in the following steps:
1): niO, mn 3 O 4 、Fe 2 O 3 And (3) respectively standing the thermal sensitive ceramic raw materials of Zn, znO, kaolin, liCl.2Al3.nH2O, hexagonal boron nitride and mullite powder for 9 hours at constant temperature and humidity, wherein the standing temperature is 23 ℃ and the relative humidity is 35%, and respectively transferring the thermal sensitive ceramic raw materials into a medicine box for sealing and preserving to obtain the ingredients for later use.
2): the weight (g) ratio is 3:1.3:1.7:1.5 weighing kaolin, liCl 2Al (OH) 3.nH2O, hexagonal boron nitride and mullite powder, and uniformly mixing to obtain an adsorption compound; weighing 7.5% of NiO and 38.5% of Mn according to weight percentage 3 O 4 、13％Fe 2 O 3 Mixing 25% of Zn, 2% of ZnO and 14% of adsorption compound to obtain a mixture; and (3) putting 250g of the mixture and 400g of deionized water into a ball mill, performing ball milling for 6 hours at a ball milling rate of 150r/min, and then putting into a 50 ℃ oven for drying for 6 hours to obtain the ball grinding material.
3): and (3) sieving the ball milling material obtained in the step (2) through a 300-mesh sieve to obtain 300-mesh ball milling materials, heating the 300-mesh ball milling materials to 800 ℃ in a bell jar furnace, and presintering for 5 hours to obtain the presintering material.
4): weighing 250g of the pre-sintered material obtained in 3) and 400g of deionized water, putting the pre-sintered material and the 400g of deionized water into a ball mill, and performing ball milling for 8 hours at a ball milling rate of 180r/min to obtain the secondary grinding material.
5): and (3) placing the second abrasive into a die, pressing the die by adopting 20N force to perform static pressure molding on the second abrasive to obtain a ceramic blank, placing the ceramic blank into a bell jar furnace, and sintering at the temperature of 1250 ℃ for 6 hours to obtain a ceramic core ingot.
6): cutting a ceramic core ingot into ceramic sheets with the thickness of 0.45mm, coating silver paste on the surfaces of the ceramic sheets, coating the ceramic sheets with the thickness of 80 mu m, and curing for 20s at the temperature of 800 ℃ to enable the ceramic sheets and the silver layers to be tightly combined for cutting, thus obtaining the thermosensitive ceramic.
Example 7
Example 7 differs from example 6 in that: the adsorption composite has different proportions of raw materials, specifically, the ratio of weight (g) is 3:1.2:1.5:1.3 weighing kaolin, liCl.2Al3.nH2O, hexagonal boron nitride and mullite powder, and uniformly mixing to obtain an adsorption compound.
Example 8
Example 8 differs from example 6 in that: the adsorption composite has different proportions of raw materials, specifically, the ratio of weight (g) is 3:1.5:1.8:1.7 weighing kaolin, liCl.2Al3.nH2O, hexagonal boron nitride and mullite powder, and uniformly mixing to obtain an adsorption compound.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that no 3) ball milling material was directly subjected to ball milling again, specifically the steps were: weighing 250g of the grinding ball material obtained in 2) and 400g of deionized water, putting the grinding ball material and the 400g of deionized water into a ball mill, and performing ball milling for 8 hours at a ball milling rate of 180r/min to obtain a secondary grinding material.
Comparative example 2
Comparative example 2 differs from example 2 in that no 4) the pre-sinter is put directly into a mold for hydrostatic molding, and the specific steps are: weighing the presintering material obtained in the step 3), placing the presintering material into a die, pressing the die by adopting 20N force to enable the presintering material to be subjected to static pressure molding, obtaining a ceramic embryo, placing the ceramic embryo into a bell jar furnace, and sintering for 6 hours at the temperature of 1250 ℃ to obtain the ceramic core ingot.
Comparative example 3
Comparative example 3 is different from example 1 in that: 3) The burn-in time in (2 h).
Comparative example 4
Comparative example 4 differs from example 1 in that: 4) The ball time in (2) was 3h.
Comparative example 5
Comparative example 5 differs from example 4 in that: the weight percentage of NiO is 25 percent, mn 3 O 4 Is 30% by weight.
Comparative example 6
Comparative example 6 differs from example 4 in that: equal amounts of Zn are replaced by ZnO.
Comparative example 7
Comparative example 7 differs from example 4 in that: mn (Mn) 3 O 4 Equivalent substitution of Al 2 O 3 。
Comparative example 8
Comparative example 8 differs from example 8 in that: liCl.2Al (OH) 3.nH2O is replaced by kaolin in equal quantity.
Comparative example 9
Comparative example 9 differs from example 8 in that: equal amounts of hexagonal boron nitride were replaced with kaolin.
Experimental test
The following performance tests were conducted on the thermosensitive ceramics obtained in examples 1 to 8 and comparative examples 1 to 9, as shown in Table 1.
1. Resistivity of
The resistivity was measured with reference to the national standard GB/T41606-2022, as shown in Table 1.
2. B value
The larger the B value is, the larger the change of the resistance value is, the more sensitive is, the B value is detected by referring to a national standard GB T7154.2-2003 direct heating type step positive temperature coefficient thermistor, and specific data are shown in a table 1;
TABLE 1 Experimental data for examples 1-8 and comparative examples 1-9
As can be seen from the combination of example 1 and comparative examples 1-2 and Table 1, the B value of example 1 is higher than that of comparative examples 1-2, indicating that the heat-sensitive ceramic obtained by the two-pass grinding of balls or by the preheating treatment has a good heat-sensitive effect.
As can be seen from the combination of examples 1 and comparative examples 3 to 4 and Table 1, the B value of example 1 is higher than that of comparative examples 3 to 4, which means that the thermosensitive effect of the thermosensitive ceramic obtained is reduced when the burn-in time is only 2 hours or the ball grinding time is only 3 hours, and further that the thermosensitive ceramic obtained by the burn-in time and the grinding time within the range of the present application is sufficiently mixed and fine, and further the thermosensitive property of the thermosensitive ceramic is improved.
Comparative example 4 and comparative example 5, example 4 has a B value higher than that of comparative example 5, indicating that NiO and Mn in the weight percent range of the present application are used 3 O 4 The heat sensitive ceramic obtained by mixing has better heat sensitivity.
Comparative examples 4 and comparative examples 6 to 7, the B values of comparative examples 6 to 7 are lower than those of example 4, indicating that when ZnO or Mn is not added 3 O 4 When the temperature-sensitive ceramic is used, the temperature-sensitive effect of the temperature-sensitive ceramic is reduced, which shows that the composition of the raw materials adopted by the application ensures that the temperature-sensitive ceramic obtains better heat sensitivity.
The B values of comparative examples 8 and 8-9 are lower than those of example 8, which shows that the ceramic core ingot prepared by compounding kaolin, liCl.2Al3.nH2O, hexagonal boron nitride and mullite powder has better compactness and further improves the thermosensitive effect of thermosensitive ceramics.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The production process of the thermosensitive ceramic is characterized by comprising the following preparation steps:
1): standing the heat sensitive ceramic raw materials for 6-9h respectively, and sealing and preserving to obtain a standby ingredient;
2): weighing the ingredients to be used respectively according to the weight percentage, mixing to obtain a mixture, mixing 200-300 parts of the mixture with 380-420 parts of water, ball milling for 4-6 hours, and drying to obtain the ball grinding material;
3): sieving the ball milling material, presintering for 4-6 hours at 700-900 ℃ to obtain presintering material;
4): mixing 200-300 parts of the mixture with 380-420 parts of water according to parts by weight, and ball milling for 7-9 hours to obtain a secondary grinding material;
5): carrying out static pressure molding on the secondary grinding material to obtain a ceramic blank, and sintering the ceramic blank at 1200-1300 ℃ for 5-7h to obtain a ceramic core ingot;
6): cutting the ceramic core ingot into ceramic sheets, coating silver paste on the surfaces of the ceramic sheets, curing at 780-850 ℃, and cutting to obtain the thermosensitive ceramic.
2. The production process of the thermosensitive ceramic according to claim 1, wherein: the raw materials of the thermosensitive ceramic comprise the following raw materials in percentage by weight:
NiO：5-9%
Mn 3 O 4 ：46-50%
Fe 2 O 3 ：13-18%
Zn：23-27%
ZnO：1-8%。
3. the production process of the thermosensitive ceramic according to claim 2, wherein the mixture of 2) is obtained by the following method: weighing NiO, mn3O4, fe2O3, zn and ZnO according to the weight percentage, and mixing to obtain the mixture.
4. The production process of the thermosensitive ceramic according to claim 1, wherein: the standing temperature in the step 1) is 23-27 ℃, and the relative humidity is 27-35%.
5. The production process of the thermosensitive ceramic according to claim 1, wherein: the ball milling rate in the steps 1) and 2) is 150-200r/min.
6. The production process of the thermosensitive ceramic according to claim 1, wherein: 3) The number of the sieves in the process is 100-800 meshes.
7. The production process of the thermosensitive ceramic according to claim 1, wherein: the thickness of the ceramic sheet is 0.40-0.50mm.
8. The production process of the thermosensitive ceramic according to claim 1, wherein: 5) The coating thickness of the silver paste is 50-100 mu m.
9. The production process of the thermosensitive ceramic according to claim 1, wherein: the raw materials of the thermosensitive ceramic comprise the following raw materials in percentage by weight:
adsorption composite 13-15%
NiO：5-9%
Mn 3 O 4 ：36-40%
Fe 2 O 3 ：10-15%
Zn：23-27%
ZnO：1-3%。
10. The production process of the thermosensitive ceramic according to claim 9, wherein: the adsorption compound is prepared from kaolin, liCl 2Al (OH) 3.nH2O, hexagonal boron nitride and mullite powder in a weight ratio of 3: (1.2-1.5): (1.5-1.8): (1.3-1.7).
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