CN115368129A - Laminated zinc oxide composition for reducing residual pressure and preparation method thereof - Google Patents

Laminated zinc oxide composition for reducing residual pressure and preparation method thereof Download PDF

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CN115368129A
CN115368129A CN202211014019.2A CN202211014019A CN115368129A CN 115368129 A CN115368129 A CN 115368129A CN 202211014019 A CN202211014019 A CN 202211014019A CN 115368129 A CN115368129 A CN 115368129A
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zinc oxide
oxide composition
calcination
reinforcing agent
residual pressure
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李吉晓
李岩
余国华
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Rudong Baolian Electronic Technology Co ltd
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Abstract

The application relates to a laminated zinc oxide composition for reducing residual pressure and a preparation method thereof, relating to the technical field of piezoresistors and comprising the following components in parts by weight: 90-100 parts of ZnO,2.1-2.5 parts of Cr 2 O 3 4.8-6.8 parts of Mn 2 O 3 3.2-4.2 parts of Co 2 O 3 1-3 parts of B 2 O 3 3.5-4.5 parts of Al 2 O 3 4-6 parts of aluminum-zinc-silicon glass and 12-16 parts of reinforcing agent. The application has the effect of improving the electrical property of the laminated zinc oxide composition.

Description

Laminated zinc oxide composition for reducing residual pressure and preparation method thereof
Technical Field
The application relates to the technical field of piezoresistors, in particular to a laminated zinc oxide composition for reducing residual voltage and a preparation method thereof.
Background
The piezoresistor has excellent nonlinear characteristics, and is widely applied to overvoltage surge protection of various electronic equipment. The multilayer chip ZnO varistor is a novel varistor produced by adopting a tape casting lamination process on the basis of the traditional varistor, has the characteristics of miniaturization, chip mounting and the like, adapts to the development trend of integration and miniaturization of electronic equipment, and is more and more widely applied. Compared with another main surge protection device transient suppression diode TVS, the chip varistor has the advantages of high energy density, stable high-temperature performance and the like, but the application of the chip varistor in the protection of a plurality of precise circuits is limited due to the higher protection voltage (residual voltage).
In view of the above application characteristics, the inventors thought that it was necessary to develop a layered zinc oxide composition for reducing residual pressure and a method for preparing the same.
Disclosure of Invention
In order to improve the electrical property of the laminated zinc oxide composition, the application provides the laminated zinc oxide composition for reducing residual pressure and the preparation method thereof.
In a first aspect, the application provides a stacked zinc oxide composition for reducing residual pressure, which adopts the following technical scheme:
a laminated zinc oxide composition for reducing residual pressure comprises the following components in parts by weight:
Figure BDA0003811949010000011
by adopting the technical scheme, cr is added 2 O 3 、Mn 2 O 3 、Co 2 O 3 Added into ZnO, effectively promotes the growth of ZnO crystal grains, and forms a high-impedance grain boundary layer between the ZnO crystal grains, thereby improving the semiconductivity of the composition; b is 2 O 3 The zinc oxide varistor material can react with ZnO, so that the uniformity of the microstructure of the zinc oxide varistor material is improved; al (Al) 2 O 3 The addition of the zinc oxide voltage dependent resistor effectively improves the electrical property stability of the zinc oxide voltage dependent resistor material; the addition of the aluminum-zinc-silicon glass can improve the low-temperature co-firing stability of the zinc oxide composition; the electrical property of the zinc oxide piezoresistor material is improved by adding the reinforcing agent.
Preferably, the reinforcing agent comprises Sb 2 O 3 And Bi 2 O 3 。
By adopting the technical scheme, sb 2 O 3 、Bi 2 O 3 Bismuth antimonic acid is generated by reacting with oxygen, and on one hand, the bismuth antimonic acid can promote growth of ZnO crystal grain size; on the other hand, the oxygen partial pressure generated during sintering is increased, and the resistivity of ZnO crystal grains is effectively increased; when bismuth antimonic acid is added into the laminated zinc oxide composition, the bismuth antimonic acid reacts with ZnO to generate a spinel phase and a bismuth-rich liquid phase, the spinel phase is pinned in a crystal boundary, the possibility of overlarge growth of ZnO crystal grains can be reduced, and the bismuth-rich liquid phase can push other materialsThe additive is uniformly distributed in ZnO crystal grains and crystal boundaries; in addition, the radius of Bi ions is far greater than that of Zn ions, so that the Bi ions cannot enter zinc oxide grains and can segregate at grain boundaries during cooling, other oxides are also segregated at the grain boundaries, the barrier potential of the grain boundaries is improved, the nonlinear coefficient of the zinc oxide pressure-sensitive ceramic is improved, and the flow capacity is improved.
Preferably, the Sb is 2 O 3 And Bi 2 O 3 The mass ratio of (1) to (2.3-2.7).
By adopting the technical scheme, sb is removed 2 O 3 And Bi 2 O 3 The mass ratio of (A) to (B) is controlled within the range, and the electrical property of the zinc oxide piezoresistor material is further improved.
Preferably, the reinforcing agent is prepared by the following method:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is uniformly mixed, and then sequentially carrying out calcination, cooling and annealing treatment to obtain the reinforcing agent.
Preferably, the calcination temperature in the preparation process of the reinforcing agent is 600-800 ℃, and the calcination time is 1.5-2.5h.
Preferably, the annealing temperature in the reinforcing agent preparation process is 400-600 ℃, and the annealing time is 1.5-2.5h.
Preferably, the composition also comprises 2-4 parts of TiO 2 。
By adopting the technical scheme, the TiO is mixed 2 Added into an accelerant, and further promotes the growth of ZnO crystal grains, thereby improving the semiconductivity of the laminated zinc oxide composition and further improving the electrical property of the zinc oxide varistor material.
In another aspect, the present application provides a method for preparing a multilayer zinc oxide composition for reducing residual pressure, comprising the steps of:
s1, mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 、Al 2 O 3 、TiO 2 Mixing the reinforcing agent and a part of ZnO, grinding and calcining to obtain the composite materialSintering materials;
s2, crushing and grinding the sintered material, and then adding aluminum-zinc-silicon glass for dispersing and mixing to prepare a zinc oxide composition preparation material;
s3, performing primary calcination on the zinc oxide composition prepared material, and levigating after the calcination is completed; then B is added 2 O 3 And the rest ZnO are evenly mixed and then are calcined for the second time, and after the calcination is finished, the mixture is crushed and ground to prepare the laminated zinc oxide composition.
By adopting the technical scheme, the zinc oxide composition is calcined for the first time to generate a pyrochlore phase, the pyrochlore phase and the residual ZnO are calcined for the second time to generate a spinel phase, and bismuth oxide is released again to promote the generation of a bismuth-rich liquid phase.
Preferably, the temperature of the primary calcination in the step S3 is 820-840 ℃, and the calcination time is 3.5-4.5h.
Preferably, the temperature of the secondary calcination in the step S3 is 900-1000 ℃, and the calcination time is 1.5-2.5h.
In summary, the present application includes at least one of the following beneficial technical effects:
1. mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 Added into ZnO, effectively promotes the growth of ZnO crystal grains, and forms a high-impedance grain boundary layer between the ZnO crystal grains, thereby improving the semiconductivity of the composition; b is 2 O 3 The zinc oxide varistor material can react with ZnO, so that the uniformity of the microstructure of the zinc oxide varistor material is improved; al (Al) 2 O 3 The addition of the zinc oxide voltage dependent resistor effectively improves the electrical property stability of the zinc oxide voltage dependent resistor material; the addition of the aluminum-zinc-silicon glass can improve the low-temperature co-firing stability of the zinc oxide composition; adding an enhancer; the electrical property of the zinc oxide piezoresistor material is improved.
2.Sb 2 O 3 、Bi 2 O 3 Bismuth antimonic acid is generated by reacting with oxygen, and on one hand, the bismuth antimonic acid can promote growth of ZnO crystal grain size; on the other hand, the oxygen partial pressure generated in the sintering process is increased, and the resistivity of ZnO crystal grains is effectively increased; when bismuth antimonic acid is added to the stackWhen the layered zinc oxide composition is used, a spinel phase and a bismuth-rich liquid phase can be generated, and the spinel phase reduces the possibility of over-large growth of ZnO crystal grains; the bismuth-rich liquid phase improves the uniformity of other additives distributed in ZnO crystal grains and crystal boundaries.
Detailed Description
Example 1
The reinforcing agent comprises the following raw materials: 10gSb 2 O 3 ，23gBi 2 O 3 。
The reinforcing agent is prepared by the following steps:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is evenly mixed, then calcining for 2.5 hours at 600 ℃, cooling after the calcining is finished, and then annealing for 2.5 hours at 400 ℃ to prepare the reinforcing agent.
The laminated zinc oxide composition comprises the following raw materials: 90gZnO,2.1gCr 2 O 3 ，4.8gMn 2 O 3 ，3.2gCo 2 O 3 ，3.5gAl 2 O 3 ，2gTiO 2 12g of reinforcing agent, 4g of aluminum-zinc-silicon glass and 1gB 2 O 3 。
A method for preparing a layered zinc oxide composition comprising the steps of:
s1, mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 、Al 2 O 3 、TiO 2 Mixing the reinforcing agent and 1/3ZnO, grinding and calcining to prepare a sintering material;
s2, crushing and grinding the sintered material, and then adding aluminum-zinc-silicon glass for dispersing and mixing to prepare a zinc oxide composition preparation material;
s3, performing primary calcination on the zinc oxide composition prepared material at 820 ℃ for 4.5 hours, and grinding after the primary calcination is completed; then B is added 2 O 3 And the rest ZnO are evenly mixed, and then the mixture is calcined for the second time at 900 ℃ for 2.5 hours, and after the second calcination is finished, the mixture is crushed and ground to prepare the laminated zinc oxide composition.
Example 2
The reinforcing agent comprisesThe following raw materials: 10gSb 2 O 3 ，27gBi 2 O 3 。
The reinforcing agent is prepared by the following steps:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is uniformly mixed, then calcining at 800 ℃ for 1.5h, cooling after the calcination is finished, and then annealing at 600 ℃ for 1.5h to prepare the reinforcing agent.
The laminated zinc oxide composition comprises the following raw materials: 100gZnO,2.5gCr 2 O 3 ，6.8gMn 2 O 3 ，4.2gCo 2 O 3 ，4.5gAl 2 O 3 ，4gTiO 2 16g of reinforcing agent, 6g of aluminum-zinc-silicon glass and 3gB 2 O 3 。
A method for preparing a layered zinc oxide composition comprising the steps of:
s1, mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 、Al 2 O 3 、TiO 2 Mixing the reinforcing agent and 1/3ZnO, grinding and calcining to prepare a sintering material;
s2, crushing and grinding the sintered material, and then adding aluminum-zinc-silicon glass for dispersing and mixing to prepare a zinc oxide composition preparation material;
s3, performing primary calcination on the zinc oxide composition preparation material at 840 ℃ for 3.5 hours, and grinding after the primary calcination is completed; then B is added 2 O 3 And the rest ZnO are evenly mixed, then the mixture is calcined for the second time for 1.5h at 1000 ℃, and after the second time calcination is finished, the mixture is crushed and ground to prepare the laminated zinc oxide composition.
Example 3
The reinforcing agent comprises the following raw materials: 10gSb 2 O 3 ，25gBi 2 O 3 。
The reinforcing agent is prepared by the following steps:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is evenly mixed, then calcining for 2 hours at 700 ℃, and after the calcining is finished, carrying outCooling, and annealing at 500 deg.C for 2 hr to obtain the reinforcing agent.
The laminated zinc oxide composition comprises the following raw materials: 95gZnO,2.3gCr 2 O 3 ，5.8gMn 2 O 3 ，3.7gCo 2 O 3 ，4gAl 2 O 3 ，3gTiO 2 14g of reinforcing agent, 5g of aluminum-zinc-silicon glass and 2gB 2 O 3 。
A method for preparing a layered zinc oxide composition, comprising the steps of:
s1, mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 、Al 2 O 3 、TiO 2 Mixing the reinforcing agent and 1/3ZnO, grinding and calcining to prepare a sintering material;
s2, crushing and grinding the sintered material, and then adding aluminum-zinc-silicon glass for dispersing and mixing to prepare a zinc oxide composition preparation material;
s3, performing primary calcination on the zinc oxide composition preparation material at 830 ℃ for 4h, and levigating after the primary calcination is completed; then B is added 2 O 3 And the rest ZnO are evenly mixed, then the mixture is calcined for the second time at 950 ℃ for 2 hours, and after the second calcination is finished, the mixture is crushed and ground to prepare the laminated zinc oxide composition.
Example 4
Example 4 differs from example 3 in that: 11.3gSb 2 O 3 ，23.7gBi 2 O 3 。
Example 5
Example 5 differs from example 3 in that: 9gSb 2 O 3 ，26gBi 2 O 3 。
Example 6
Example 6 differs from example 3 in that: 1gTiO 2 2 。
Example 7
Example 7 differs from example 3 in that: 5gTiO 2 2 。
Example 8
Example 8 differs from example 3 in that: the reinforcing agent is prepared by the following steps:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is uniformly mixed, then calcining for 2 hours at 500 ℃, cooling after the calcining is finished, and then annealing for 2 hours at 500 ℃ to prepare the reinforcing agent.
Example 9
Example 9 differs from example 3 in that: the reinforcing agent is prepared by the following steps:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is uniformly mixed, then calcining for 2 hours at 900 ℃, cooling after the calcining is finished, and then annealing for 2 hours at 500 ℃ to prepare the reinforcing agent.
Comparative example 1
Comparative example 1 and example 3 differ in that: a method for preparing a layered zinc oxide composition comprising the steps of:
s1, mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 、Al 2 O 3 、TiO 2 、Sb 2 O 3 、Bi 2 O 3 Mixing with 1/3ZnO, grinding and calcining to prepare a sintering material;
s2, crushing and grinding the sintered material, and then adding aluminum-zinc-silicon glass for dispersing and mixing to prepare a zinc oxide composition preparation material;
s3, performing primary calcination on the zinc oxide composition preparation material at 830 ℃ for 4h, and levigating after the primary calcination is completed; then B is added 2 O 3 And the rest ZnO are evenly mixed, then the mixture is calcined for the second time at 950 ℃ for 2 hours, and after the second calcination is finished, the mixture is crushed and ground to prepare the laminated zinc oxide composition.
Comparative example 2
Comparative example 2 and example 3 differ in that: 35gSb 2 O 3 ，0gBi 2 O 3 。
Comparative example 3
Comparative example 3 differs from example 3 in that:0gSb 2 O 3 ，35gBi 2 O 3 。
comparative example 4
Comparative example 4 differs from example 3 in that: the laminated zinc oxide composition does not contain TiO 2 。
And (3) performance testing: the laminated zinc oxide compositions prepared in examples 1 to 9 and comparative examples 1 to 4 were pressed into a wafer having a diameter of 20mm and a thickness of 6mm under a pressure of 100Mpa, and then sintered at 860 ℃ for 4 hours to prepare zinc oxide pressure sensitive material samples, 10 samples were prepared for each of the examples and comparative examples, and the average values of the electrical property test results of the samples were as shown in table 1.
TABLE 1
Figure BDA0003811949010000061
As can be seen from table 1, the breakdown voltage of the zinc oxide pressure sensitive materials prepared from the stacked zinc oxide compositions of examples 1 to 3 is 1020 to 1052.3V, the voltage gradient is 340 to 345V/mm, the non-linearity index α is 91 to 94, the leakage current is 0.85 to 0.89 μ a, and the residual voltage ratio is 1.32 to 1.37V/mm, so that the stacked zinc oxide compositions of the present application have better electrical properties and lower residual voltage characteristics.
As can be seen from table 1, example 4 differs from example 3 in that: example 3 10gSb 2 O 3 ，25gBi 2 O 3 11.3gSb in example 4 2 O 3 ，23.7gBi 2 O 3 (ii) a Example 4 showed a significant decrease in electrical properties and a significant increase in residual voltage ratio as compared with example 3, because Bi was added 2 O 3 When the content of (a) is reduced, on the one hand, the amount of the generated bismuth antimonic acid is reduced, so that the promotion effect on ZnO crystal grains is reduced; on the other hand, the amount of the generated bismuth-rich solution is reduced, so that the dispersion uniformity of other additives in ZnO crystal grains and crystal boundaries is reduced, the density of the generated zinc oxide piezoresistor is reduced, and the electrical property and the residual voltage property of the laminated zinc oxide composition are reduced.
As can be seen from Table 1, examples 5 and 5The differences of 3 are that: example 3 10gSb 2 O 3 ，25gBi 2 O 3 9gSb in example 5 2 O 3 ，26gBi 2 O 3 (ii) a In example 5, the electrical properties are significantly reduced and the residual voltage ratio is significantly increased compared to example 3, because when Bi is added 2 O 3 When the content of (B) increases, free Bi 2 O 3 Can directly generate a spinel phase with ZnO, so that the inhibition effect on the growth of ZnO crystal grains is overlarge, the density of the generated zinc oxide piezoresistor is reduced, and the electrical property and the residual voltage property of the laminated zinc oxide composition are reduced.
As can be seen from table 1, example 6 differs from example 3 in that: example 3 the composition of the layered zinc oxide contains 3gTiO 2 In example 6, the layered zinc oxide composition contained 1g of TiO 2 (ii) a Example 6 showed a significant decrease in electrical properties and a significant increase in residual voltage ratio as compared to example 3, because TiO significantly decreased residual voltage when compared to the same material 2 When the content of (B) is reduced, tiO is obtained 2 The promotion effect on the growth of ZnO crystal grains is weakened, so that a grain boundary layer formed among the ZnO crystal grains becomes thinner, and the electrical property and the residual voltage property of the laminated zinc oxide composition are reduced.
As can be seen from table 1, example 7 differs from example 3 in that: example 3 the composition of the layered zinc oxide contains 3gTiO 2 Example 7 the composition of the layered zinc oxide contained 5g of TiO 2 (ii) a Example 7 showed a significant decrease in electrical properties and a significant increase in residual voltage ratio as compared with example 3, because TiO significantly decreased the residual voltage ratio 2 When the content of (a) is increased, znO crystal grains grow abnormally, the microstructure of the ZnO crystal grains is not uniform, and pores exist in the ZnO crystal grains, so that the electrical property of the laminated zinc oxide composition is reduced, and the residual voltage characteristic is improved.
As can be seen from table 1, example 8 differs from example 3 in that: the calcination temperature of the reinforcing agent in example 3 is 700 ℃, and the calcination temperature of the reinforcing agent in example 8 is 500 ℃; example 8 showed a significant decrease in electrical properties and a significant increase in residual pressure ratio as compared with example 3, because Sb was caused to be Sb when the calcination temperature of the reinforcing agent was lowered 2 O 3 And Bi 2 O 3 Calcination ofThe produced reinforcing agent contains other impurities incompletely, so that the density of the produced zinc oxide piezoresistor is reduced, and the electrical property and residual voltage property of the laminated zinc oxide composition are reduced.
As can be seen from table 1, example 9 differs from example 3 in that: as can be seen from table 1, example 8 differs from example 3 in that: the calcination temperature of the reinforcing agent in example 3 was 700 ℃ and the calcination temperature of the reinforcing agent in example 9 was 900 ℃; example 9 showed a significant decrease in electrical properties and a significant increase in residual pressure ratio as compared with example 3, because Sb may be caused when the calcination temperature of the reinforcing agent is increased 2 O 3 And Bi 2 O 3 The promoting effect of the generated bismuth antimonic acid on the growth of ZnO crystal grains is weakened, so that the density of the generated zinc oxide piezoresistor is reduced, the electrical property of the laminated zinc oxide composition is reduced, and the residual voltage characteristic is improved.
As can be seen from table 1, comparative example 1 and example 3 differ in that: in example 3 Sb is first introduced 2 O 3 And Bi 2 O 3 Forming a reinforcing agent, adding the reinforcing agent into the laminated zinc oxide composition, and directly adding Sb into the laminated zinc oxide composition in comparative example 1 2 O 3 And Bi 2 O 3 Directly adding the zinc oxide powder into a laminated zinc oxide composition for calcination; comparative example 1 and example 3 showed a significant drop in electrical properties and a significant increase in residual voltage ratio, because Sb 2 O 3 And Bi 2 O 3 The bismuth antimonite can not be generated because the pyrochlore phase is directly reacted with ZnO and the spinel phase is generated, thereby the promotion effect on ZnO crystal grains is weakened, the density of the generated zinc oxide piezoresistor is reduced, and the electrical property and the residual voltage characteristic of the laminated zinc oxide composition are reduced.
As can be seen from table 1, comparative example 2 and example 3 differ in that: example 3 10gSb 2 O 3 ，25gBi 2 O 3 35gSb in example 4 2 O 3 ，0gBi 2 O 3 (ii) a Comparative example 2 shows a significant decrease in electrical properties and a significant increase in residual voltage ratio as compared with example 3, because the reinforcing agent does not contain Bi 2 O 3 On the one hand, it is impossibleBismuth antimonic acid is generated, so that the promotion effect on ZnO crystal grains is weakened; on the other hand, a spinel phase cannot be generated, and the abnormal growth of ZnO crystal grains cannot be inhibited, so that the density and the microstructure uniformity of the generated zinc oxide piezoresistor are reduced, and the electrical property and the residual voltage property of the laminated zinc oxide composition are reduced.
As can be seen from table 1, comparative example 3 differs from example 3 in that: example 3 10gSb 2 O 3 ，25gBi 2 O 3 0g Sb in example 4 2 O 3 ，35gBi 2 O 3 (ii) a Comparative example 3 has a significant decrease in electrical properties and a significant increase in residual voltage ratio as compared to example 3, because no Sb is contained in the reinforcing agent 2 O 3 On one hand, bismuth antimonic acid cannot be generated, so that the promotion effect on ZnO crystal grains is weakened; on the other hand, spinel phase can not be generated, and the inhibition effect on abnormal growth of ZnO crystal grains can not be achieved, so that the density and microstructure uniformity of the generated zinc oxide piezoresistor are reduced, and the electrical property and residual voltage characteristic of the laminated zinc oxide composition are reduced.
As can be seen from table 1, comparative example 4 differs from example 3 in that: example 3 Accelerator containing TiO 2 Comparative example 2, which does not contain TiO 2 (ii) a The electrical properties are significantly reduced compared to example 2 and example 3, since no TiO is contained in the promoter 2 Effectively reducing the promotion effect on the growth of ZnO crystal grains, thereby reducing the electrical property of the laminated zinc oxide composition and improving the residual voltage characteristic.
The present embodiment is merely illustrative, and not restrictive, and various changes and modifications may be made by persons skilled in the art without departing from the scope and spirit of the present invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.

Claims (10)

1. A laminated zinc oxide composition for reducing residual pressure, comprising: the paint comprises the following components in parts by weight:
90-100 parts of ZnO
Cr 2 O 3 2.1 to 2.5 portions
Mn 2 O 3 4.8 to 6.8 portions of
Co 2 O 3 3.2 to 4.2 portions of
B 2 O 3 1 to 3 portions of
Al 2 O 3 3.5 to 4.5 portions of
4-6 parts of aluminum-zinc-silicon glass
12-16 parts of a reinforcing agent.
2. The residual pressure reducing layered zinc oxide composition according to claim 1, wherein: the reinforcing agent comprises Sb 2 O 3 And Bi 2 O 3 。
3. The stacked zinc oxide composition of claim 2, wherein: the Sb 2 O 3 And Bi 2 O 3 The mass ratio of (1) to (2.3-2.7).
4. The stacked zinc oxide composition of claim 2, wherein: the reinforcing agent is prepared by the following method:
sb 2 O 3 And Bi 2 O 3 After mixing, grinding until the mixture is uniformly mixed, and then sequentially carrying out calcination, cooling and annealing treatment to obtain the reinforcing agent.
5. The residual pressure reducing layered zinc oxide composition according to claim 4, wherein: the calcination temperature in the preparation process of the reinforcing agent is 600-800 ℃, and the calcination time is 1.5-2.5h.
6. The residual pressure reducing layered zinc oxide composition according to claim 4, wherein: the annealing temperature in the preparation process of the reinforcing agent is 400-600 ℃, and the annealing time is 1.5-2.5h.
7. The residual pressure reducing layered zinc oxide composition according to claim 4, wherein: the composition also comprises 2-4 parts of TiO 2 。
8. A method of making the reduced residual pressure layered zinc oxide composition of claim 7, wherein: the method comprises the following steps:
s1, mixing Cr 2 O 3 、Mn 2 O 3 、Co 2 O 3 、Al 2 O 3 、TiO 2 Mixing the reinforcing agent and a part of ZnO, grinding and calcining to prepare a sintering material;
s2, crushing and grinding the sintered material, and then adding aluminum-zinc-silicon glass for dispersing and mixing to prepare a zinc oxide composition preparation material;
s3, performing primary calcination on the zinc oxide composition prepared material, and levigating after the calcination is completed; then B is added 2 O 3 And the rest ZnO are evenly mixed and then are calcined for the second time, and after the calcination is finished, the mixture is crushed and ground to prepare the laminated zinc oxide composition.
9. The method of claim 8 for preparing a reduced residual pressure layered zinc oxide composition, wherein: the temperature of the primary calcination in the step S3 is 820-840 ℃, and the calcination time is 3.5-4.5h.
10. The method of claim 8 for preparing a reduced residual pressure layered zinc oxide composition, wherein: the temperature of the secondary calcination in the step S3 is 900-1000 ℃, and the calcination time is 1.5-2.5h.
CN202211014019.2A 2022-08-23 2022-08-23 Laminated zinc oxide composition for reducing residual pressure and preparation method thereof Pending CN115368129A (en)

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