CN108439970A - A kind of compound thermal sensitive ceramic material of Rare Earth Doped Perovskite NTC and preparation method - Google Patents
A kind of compound thermal sensitive ceramic material of Rare Earth Doped Perovskite NTC and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC and preparation method, the chemical formula of the ceramic material to be：(1‑x)BBF‑xY2O3, wherein the value range of x is 0.01 0.2.The BBF powders are the Bi that purity is 99.63%2O3Powder, the BaCO that purity is 99.5%3Powder, the Fe that purity is 99.5%2O3Powder.The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC are made with two step solid-phase synthesis in this method.The invention has the advantages that the method for the present invention is by controlling BBF and Y2O3Component ratio, the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC, which may be implemented, has coexisting compared with low-resistance value and the quick constant B values of higher thermal, provides convenience for the wide warm area application of such material.
Description
Technical field
The present invention relates to a kind of compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC and preparation methods.
Background technology
Negative temperature coefficient (Negative Temperature Coefficient, abbreviation NTC) resistor is a quasi-resistance
The sensing element exponentially reduced is increased with temperature, with higher sensitivity, response is fast, interchangeability is good, small and cost
Low advantage is widely used in the equipment such as temperature measurement, temperature control, temperature-compensating and voltage stabilizing.Currently, widely used
Polynary spinel structure (the AB that NTC thermistors are mainly made of elements such as Mn, Ni, Cu, Co2O4) material system.Spinelle
The tetrahedron and octahedral cations of structure NTC thermal sensitive ceramicses can be redistributed slowly at any time when temperature is more than 473K,
Lead to structure relaxation phenomenon, affect the stability of material, and limits the use temperature range of such material.And calcium titanium
Mine type thermal sensitive ceramics structure has good temperature stability, preferably to be applied under wide temperature environment, therefore Ca-Ti ore type
NTC thermal sensitive ceramicses are concerned, and become one of the research hotspot of NTC thermo-sensitive materials.
In addition, NTC thermal sensitive ceramic materials high resistance and high temperature-sensitive constant B values exist simultaneously, it is difficult to realize high resistant, low B
Value or low-resistance, high B values coexist, but wide warm area NTC themistor requires the height of resistance value and B values to have various combination,
This is one of the technical barrier of current this field main attack.
Invention content
To solve the above-mentioned problems, it is an object of the invention to provide a kind of simple for process, calcium is prepared for by solid-phase synthesis
Titanium ore type Bi0.5Ba0.5FeO3(BBF)-Y2O3Compound NTC thermal sensitive ceramicses find to realize low-resistance by changing component and its ratio
The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC and preparation method that value and high temperature-sensitive constant B are worth coexisting.
The technical scheme is that：A kind of compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC, the ceramic material
Chemical formula be：(1-x)BBF-xY2O3, wherein the value range of x is 0.01-0.2.
Further, the BBF powders are the Bi that purity is 99.63%2O3Powder, the BaCO that purity is 99.5%3Powder,
The Fe that purity is 99.5%2O3Powder.
Another object of the present invention provides a kind of preparation of above-mentioned compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC
Method, this method specifically include following steps：
BBF powders after step 1. synthesis:First by Bi2O3,BaCO3And Fe2O3Powder weighs respectively according to mass ratio, so
After be put into togerther planetary mills and carry out ball milling in anhydrous ethanol medium, Ball-milling Time is 12-18 hour, is 700-900 in temperature
At DEG C pre-burning 1-3 hours to get to BBF powders, it is spare；
Step 2：By the BBF powders and Y after synthesis2O3Ball milling 15-18 hours in ball mill are proportionally added together, so
After dry to get to the compound thermal sensitive ceramics material powders of Rare Earth Doped Perovskite NTC.
Step 3：By step 2 be prepared the compound thermal sensitive ceramic material powders of Rare Earth Doped Perovskite NTC make of PVA it is viscous
Knot agent is pressed into the disk of 15mm diameters on dry-pressing formed machine, is sintered 2 hours at 1100 DEG C after plastic removal.
Further, the Bi2O3,BaCO3And Fe2O3The mass ratio of powder three is：0.5： 0.5：1.
Further, the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC have low resistance and high temperature-sensitive constant B
It is worth coexisting.
The test of ceramics sample
Using wideband dielectric/impedance analyzer to (1-x) BBF-xY2O3Ceramics sample carries out under different temperatures and frequency
Electrical performance testing.The electric property result of test is as shown in Figure 1, 2.
Ceramics sample performance evaluation
The relationship between structure and performance by analyzing different component (x=0.0,0.05,0.10,0.15,0.20), can
To analyze regulation and control of the component to performance, the regulation and control of component, structure on performance may be implemented by changing material component, and realize low
Resistance value and high temperature-sensitive constant B are worth coexisting.
The beneficial effects of the invention are as follows：Material system proposed by the invention is, it can be achieved that the height that common material is not realized
Temperature-sensitive constant and low resistance must coexist., it can be achieved that requirement of the wide warm area to NTC thermo-sensitive materials compared with general material.
Description of the drawings
Fig. 1 is the D.C. resistance variation with temperature of the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC of the present invention
Curve synoptic diagram.
Fig. 2 is the present invention (1-x) BBF-xY2O3Complex impedance spectra schematic diagram under ceramic room temperature.
Fig. 3 is the present invention (1-x) BBF-xY2O3The schematic equivalent circuit of impedance analysis under ceramic room temperature.
Specific implementation mode
Technical scheme of the present invention is described further with reference to specific embodiment.
A kind of compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC of the present invention, the chemical formula of the ceramic material are：
(1-x)BBF-xY2O3, wherein the value range of x is 0.01-0.2.
Further, the BBF powders are the Bi that purity is 99.63%2O3Powder, the BaCO that purity is 99.5%3Powder,
The Fe that purity is 99.5%2O3Powder.
Another object of the present invention provides a kind of preparation of above-mentioned compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC
Method, this method specifically include following steps：
BBF powders after step 1. synthesis:First by Bi2O3,BaCO3And Fe2O3Powder weighs respectively according to mass ratio, so
After be put into togerther planetary mills and carry out ball milling in anhydrous ethanol medium, Ball-milling Time is 12-18 hour, is 700-900 in temperature
At DEG C pre-burning 1-3 hours to get to BBF powders, it is spare；℃
Step 2：By the BBF powders and Y after synthesis2O3Ball milling 15-18 hours in ball mill are proportionally added together, so
After dry to get to the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC.
Step 3：The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC are prepared in step 2 and make binder with PVA
It is pressed into the disk of 15mm diameters on dry-pressing formed machine, is sintered 1.5-2.5 hours at 1000-1200 DEG C after plastic removal.Sintering
Sample polishing both surfaces after it is two-sided coat silver paste, then at 850 DEG C sintering after twenty minutes become electrode.
Further, the Bi2O3,BaCO3And Fe2O3The mass ratio of powder three is：0.5： 0.5：1.
Further, the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC have low resistance and high temperature-sensitive constant B
It is worth coexisting.
Embodiment 1：
(1-x)BBF-xY2O3Ceramics are synthetically prepared using the solid-phase synthesis of two steps, and high pure raw material used includes：
Bi2O3(99.63%), BaCO3(99.5%), Fe2O3(99.5%) and Y2O3(99.9%).
First, Bi2O3,BaCO3And Fe2O3By the stoichiometric ratio 0.5 of BBF ceramics：0.5：1 is matched, and is then placed in
Planetary mills carry out ball milling 16 hours in absolute ethyl alcohol, and ball-milling medium is ZrO2Ball.After dry materials after ball milling at 800 DEG C
Pre-burning is synthesized for 2 hours.BBF powders after synthesis again with the Y of different ratio2O3(molar percentage is respectively：0.05%)
Then ball milling 16 hours together are dried to get to the compound thermal sensitive ceramic material powders of Rare Earth Doped Perovskite NTC
The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC will be prepared and make binder dry-pressing formed with PVA
It is pressed into the disk of 15mm diameters on machine, is sintered 2 hours at 1100 DEG C after plastic removal, Rare Earth Doped Perovskite NTC compound thermals
Sensitive ceramic material.
Embodiment 2
(1-x)BBF-xY2O3Ceramics are synthetically prepared using the solid-phase synthesis of two steps, and high pure raw material used includes：
Bi2O3(99.63%), BaCO3(99.5%), Fe2O3(99.5%) and Y2O3(99.9%).
First, Bi2O3,BaCO3And Fe2O3By the stoichiometric ratio 0.5 of BBF ceramics：0.5：1 is matched, and is then placed in
Planetary mills carry out ball milling 12 hours in absolute ethyl alcohol, and ball-milling medium is ZrO2Ball.After dry materials after ball milling at 700 DEG C
Pre-burning is synthesized for 1 hour.BBF powders after synthesis again with the Y of different ratio2O3(molar percentage is respectively：0.10%)
Then ball milling 18 hours together are dried to get to the compound thermal sensitive ceramic material powders of Rare Earth Doped Perovskite NTC；
The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC will be prepared and make binder dry-pressing formed with PVA
It is pressed into the disk of 15mm diameters on machine, is sintered 1.5 hours at 1000 DEG C after plastic removal, Rare Earth Doped Perovskite NTC is compound
Thermal sensitive ceramic material.
Embodiment 3
(1-x)BBF-xY2O3Ceramics are synthetically prepared using the solid-phase synthesis of two steps, and high pure raw material used includes：
Bi2O3(99.63%), BaCO3(99.5%), Fe2O3(99.5%) and Y2O3(99.9%).
First, Bi2O3,BaCO3And Fe2O3By the stoichiometric ratio 0.5 of BBF ceramics：0.5：1 is matched, and is then placed in
Planetary mills carry out ball milling 14 hours in absolute ethyl alcohol, and ball-milling medium is ZrO2Ball.After dry materials after ball milling at 750 DEG C
Pre-burning is synthesized for 2 hours.BBF powders after synthesis again with the Y of different ratio2O3(molar percentage is respectively：0.15%)
Then ball milling 15 hours together are dried to get to the compound thermal sensitive ceramic material powders of Rare Earth Doped Perovskite NTC；
The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC will be prepared and make binder dry-pressing formed with PVA
It is pressed into the disk of 15mm diameters on machine, is sintered 2.5 hours at 1200 DEG C after plastic removal, Rare Earth Doped Perovskite NTC is compound
Thermal sensitive ceramic material.
Embodiment 4
(1-x)BBF-xY2O3Ceramics are synthetically prepared using the solid-phase synthesis of two steps, and high pure raw material used includes：
Bi2O3(99.63%), BaCO3(99.5%), Fe2O3(99.5%) and Y2O3(99.9%).
First, Bi2O3,BaCO3And Fe2O3By the stoichiometric ratio 0.5 of BBF ceramics：0.5：1 is matched, and is then placed in
Planetary mills carry out ball milling 16 hours in absolute ethyl alcohol, and ball-milling medium is ZrO2Ball.After dry materials after ball milling at 900 DEG C
Pre-burning is synthesized for 3 hours.BBF powders after synthesis again with the Y of different ratio2O3(molar percentage is respectively：0.20%)
Then ball milling 15.5 hours together are dried to get to the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC,
The compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC will be prepared and make binder dry-pressing formed with PVA
It is pressed into the disk of 15mm diameters on machine, is sintered 2.5 hours at 1050 DEG C after plastic removal, Rare Earth Doped Perovskite NTC is compound
Thermal sensitive ceramic material.
The test of ceramics sample
Silver paste is coated by two-sided after the polishing both surfaces of the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC, is then existed
850 DEG C of sintering become electrode after twenty minutes, using wideband dielectric/impedance analyzer to (1-x) BBF-xY2O3Ceramics sample carries out
Electrical performance testing under different temperatures and frequency.The electric property result of test is as shown in Figure 1, 2.
Ceramics sample performance evaluation
The relationship between structure and performance by analyzing different component (x=0.0,0.05,0.10,0.15,0.20), can
To analyze regulation and control of the component to performance, the regulation and control of component, structure on performance may be implemented by changing material component, and realize low
Resistance value and high temperature-sensitive constant B are worth coexisting.
Mixture after the compound thermal sensitive ceramic material drying of above-mentioned Rare Earth Doped Perovskite NTC is made into binder with PVA
The disk of 15mm diameters is pressed on dry-pressing formed machine.It is sintered 2 hours at 1100 DEG C after plastic removal.It throws on the sample two sides of sintering
Two-sided after light to coat silver paste, then at 850 DEG C, sintering is used as electrode after twenty minutes.
Structure is analyzed by XRD diffractive technologies and SEM methods, using wideband impedance analyzer to different temperatures
With under frequency resistance and the electrical parameters such as impedance be tested characterization, obtained the influence of component and structure to electric property
Rule utilizes the resistance value and formula under obtained different temperatures：B values are calculated, are found
(1-x)BBF-xY2O3The achievable low resistance of ceramics and high temperature-sensitive constant B are worth coexisting.
Influence relationship of the microstructure to electric parameters is established, it is found that grain boundary resistance is greater than grain resistance, crystal boundary
Resistance Influence bigger of the resistance to ceramics.It is demonstrated experimentally that resistance value and temperature-sensitive constant B values can be realized by the change of grain size
It must regulate and control.
Claims (5)
1. a kind of compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC, which is characterized in that the chemical formula of the ceramic material
For：(1-x)BBF-xY2O3, wherein the value range of x is 0.01-0.2.
2. ceramic material according to claim 1, which is characterized in that the BBF powders are the Bi that purity is 99.63%2O3
Powder, the BaCO that purity is 99.5%3Powder, the Fe that purity is 99.5%2O3Powder.
3. a kind of method preparing the ceramic material as described in claim 1-2 any one, which is characterized in that this method has
Body includes the following steps：
BBF powders after step 1. synthesis:First by Bi2O3, BaCO3And Fe2O3Powder weighs respectively according to mass ratio, so
After be put into togerther planetary mills and carry out ball milling in anhydrous ethanol medium, Ball-milling Time is 12-18 hour, is 700-900 in temperature
At DEG C pre-burning 1-3 hours to get to BBF powders, it is spare；
Step 2：By the BBF powders and Y after synthesis2O3Ball milling 15-18 hours in ball mill are proportionally added together, then dry
It is dry to get to the compound thermal sensitive ceramic material powders of Rare Earth Doped Perovskite NTC；
Step 3：The compound thermal sensitive ceramic material powders of Rare Earth Doped Perovskite NTC are prepared in step 2 and make binder with PVA
The disk of 15mm diameters is pressed on dry-pressing formed machine, sintering 1.5-2.5 is small at being 1000-1200 DEG C in temperature after plastic removal
When to get to the compound thermal sensitive ceramic materials of Rare Earth Doped Perovskite NTC.
4. according to the method described in claim 3, it is characterized in that, the step a kind Bi2O3, BaCO3And Fe2O3Powder three
The molar ratio of person is：0.5：0.5：1 .
5. according to the method described in claim 3, it is characterized in that, the compound thermal sensitive ceramicses of Rare Earth Doped Perovskite NTC
There is material low resistance and high temperature-sensitive constant B to be worth coexisting.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402521A (en) * | 2008-10-31 | 2009-04-08 | 桂林电子科技大学 | NTC heat-sensitive conductive ceramic material and method of manufacturing the same |
| CN102964119A (en) * | 2012-11-20 | 2013-03-13 | 桂林电子科技大学 | Low-temperature-sintered BiFeO3-based high-performance negative-temperature-coefficient thermosensitive ceramic material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402521A (en) * | 2008-10-31 | 2009-04-08 | 桂林电子科技大学 | NTC heat-sensitive conductive ceramic material and method of manufacturing the same |
| CN102964119A (en) * | 2012-11-20 | 2013-03-13 | 桂林电子科技大学 | Low-temperature-sintered BiFeO3-based high-performance negative-temperature-coefficient thermosensitive ceramic material and preparation method thereof |
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