CN114773055B - Preparation method of zirconia ceramic capable of efficiently absorbing power frequency electromagnetic field - Google Patents
Preparation method of zirconia ceramic capable of efficiently absorbing power frequency electromagnetic field Download PDFInfo
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- CN114773055B CN114773055B CN202210571514.7A CN202210571514A CN114773055B CN 114773055 B CN114773055 B CN 114773055B CN 202210571514 A CN202210571514 A CN 202210571514A CN 114773055 B CN114773055 B CN 114773055B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000000919 ceramic Substances 0.000 title claims abstract description 72
- 230000005672 electromagnetic field Effects 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000011268 mixed slurry Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 229920003257 polycarbosilane Polymers 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 31
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000002612 dispersion medium Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000001272 pressureless sintering Methods 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 238000005452 bending Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000011224 oxide ceramic Substances 0.000 description 6
- 238000000197 pyrolysis Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000004040 coloring Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical group [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
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Abstract
A preparation method of zirconia ceramics for efficiently absorbing power frequency electromagnetic fields relates to a preparation method of zirconia ceramics. The invention aims to solve the problems that most of the existing zirconia ceramics dyed by metal ions have poor effect and influence the electromagnetic performance and the heat conductivity of the ceramic body. The preparation method comprises the following steps: 1. uniformly mixing the mixed slurry; 2. drying; 3. and (4) molding and sintering. The invention is used for preparing the zirconia ceramics which can efficiently absorb the power frequency electromagnetic field.
Description
Technical Field
The invention relates to a preparation method of zirconia ceramics.
Background
With the progress of the technical field and the improvement of the living standard of people, zirconia ceramic mobile phone back plates with good mechanical property, skin-friendly texture and biocompatibility are more and more pursued. In addition, the zirconia mobile phone back plate also has good wave-transmitting performance in a (2-6 GHz) frequency band, and the application of the 5G era is very met. However, it is difficult to impart uniform color to the zirconia ceramic by the conventional method.
At present, it is common practice to soak a pre-fired, non-dense ceramic body in a solution containing metal ions, and to wick the metal ions into the matrix. Although such practices are simple, quick, and easy to regulate, these saline solutions tend to be toxic, and many studies have demonstrated that prolonged exposure to saline solutions can pose a significant health hazard to first-line workers.
In addition, most of zirconia ceramics dyed by metal ions have poor effect and influence on the electromagnetic property and the heat-conducting property of the ceramic body, so that the application of a SiC-YSZ system in the fields of mobile phone backboards and mobile wearable devices is limited.
Disclosure of Invention
The invention aims to solve the problems that most of the existing zirconia ceramics dyed by metal ions have poor effect and influence the electromagnetic performance and the heat conductivity of the ceramic body, and further provides a preparation method of the zirconia ceramics capable of efficiently absorbing power frequency electromagnetic field.
A preparation method of zirconia ceramics for efficiently absorbing power frequency electromagnetic fields comprises the following steps:
1. weighing and mixing 95-99.6 parts of yttria-stabilized zirconia, 1-20 parts of polycarbosilane solution with the mass percent of 10-20%, 0.1-0.5 part of sintering aid, 0.2-2 parts of dispersant and 0.3-1.5 parts of cross-linking agent according to the mass parts to obtain uniformly mixed slurry;
2. drying the uniformly mixed slurry at the temperature of 100-140 ℃ to obtain a dried mixed blank;
3. crushing and sieving the dried mixed blank to obtain powder with the grain size of 10-20 microns, and performing compression molding and sintering on the powder with the grain size of 10-20 microns to obtain the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field.
The invention has the beneficial effects that:
1. simple and quick: only a small amount of polycarbosilane and zirconia powder are mixed uniformly, and the presintered blank is not required to be soaked in a salt solution.
2. Safe and reliable: the polycarbosilane precursor and the zirconia powder are nontoxic and harmless, and the whole process prevents the participation of toxic metal ion solution from the source, thereby fundamentally ensuring the human health of operators.
3. The mode of mixing the polycarbosilane solution and the zirconia powder can conveniently and efficiently obtain the ceramic powder which is uniformly mixed.
4. The Polycarbosilane (PCS) is used for coloring the oxide ceramic, fills the gap of the PCS applied in the civil market in the field, and simultaneously makes the zirconia ceramic blacken and toughens the zirconia ceramic.
5. Considering the specific application of the SiC-YSZ binary ceramic, the electromagnetic absorption performance and the heat conduction performance of the SiC-YSZ ceramic are researched in a targeted manner, and on the basis of keeping the good heat conduction performance (the heat conduction performance reaches 2.2W/mK) and the wave transmission performance (the dielectric loss and the loss tangent of the ceramic are close to zero) of the YSZ ceramic, the coloring capacity and the toughness (the fracture toughness can reach 6.5MPa m at most) of the YSZ ceramic are enhanced 1/2 ) The application of the mobile phone backboard and the wearable mobile electronic equipment is expanded.
6. The application value and the potential of SiC related materials in the civil market are greatly expanded.
The invention relates to a preparation method of zirconia ceramics for efficiently absorbing a power frequency electromagnetic field.
Drawings
FIG. 1 is an element distribution diagram, wherein a is powder with a particle size of 10 μm to 20 μm prepared in the third step of the example, and b is a section of the zirconia ceramic with high efficiency of absorbing the power frequency electromagnetic field prepared in the first step of the example;
FIG. 2 is an XRD spectrum of a zirconia ceramic with different SiC contents and capable of efficiently absorbing power frequency electromagnetic field, wherein 1 is an example I, 2 is an example II, 3 is an example III, 4 is an example IV, 5 is an example V, 6 is an example VI, 7 is an example VII, 8 is 3YSZ,. Diamond-solid is t-ZrO 2 96795 is m-ZrO 2 ，
Is beta-SiC;
FIG. 3 is a graph comparing hardness and bending strength of zirconia ceramics with different SiC contents and capable of efficiently absorbing power frequency electromagnetic fields, wherein a is hardness and b is bending strength;
FIG. 4 is a graph showing the comparison of fracture toughness of zirconia ceramics with different SiC contents and high efficiency of absorbing power frequency electromagnetic field;
FIG. 5 is a wave-absorbing property diagram of the zirconia ceramic prepared in the fifth embodiment, which efficiently absorbs a power frequency electromagnetic field;
FIG. 6 is a comparison graph of the heat conductivity of zirconia ceramics with different SiC contents and capable of efficiently absorbing power frequency electromagnetic fields;
FIG. 7 is a schematic diagram of zirconia ceramics capable of efficiently absorbing power frequency electromagnetic fields prepared in example three and example five, wherein a is example three, and b is example five.
Detailed Description
The first embodiment is as follows: the embodiment provides a preparation method of zirconia ceramic for efficiently absorbing power frequency electromagnetic field, which comprises the following steps:
1. weighing and mixing 95-99.6 parts of yttria-stabilized zirconia, 1-20 parts of polycarbosilane solution with the mass percent of 10% -20%, 0.1-0.5 part of sintering aid, 0.2-2 parts of dispersant and 0.3-1.5 parts of cross-linking agent in parts by mass to obtain uniformly mixed slurry;
2. drying the uniformly mixed slurry at the temperature of 100-140 ℃ to obtain a dried mixed blank;
3. crushing and sieving the dried mixed blank to obtain powder with the grain size of 10-20 microns, and performing compression molding and sintering on the powder with the grain size of 10-20 microns to obtain the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field.
The polycarbosilane described in the present embodiment is a precursor of a functional pigment.
The beneficial effects of the embodiment are as follows:
1. simple and quick: only a small amount of polycarbosilane is required to be uniformly mixed with zirconia powder, and the pre-sintered blank is not required to be soaked into a salt solution.
2. Safe and reliable: the polycarbosilane precursor and the zirconia powder are nontoxic and harmless, and the whole process prevents the participation of toxic metal ion solution from the source, thereby fundamentally ensuring the human health of operators.
3. The mode of mixing the polycarbosilane solution and the zirconia powder can conveniently and efficiently obtain the ceramic powder which is uniformly mixed.
4. The Polycarbosilane (PCS) is used for coloring the oxide ceramic, fills the gap of the PCS applied in the civil market in the field, and simultaneously makes the zirconia ceramic blacken and toughens the zirconia ceramic.
5. Considering the specific application of the SiC-YSZ binary ceramic, the electromagnetic absorption performance and the heat conduction performance of the SiC-YSZ ceramic are researched in a targeted manner, and on the basis of maintaining the good heat conduction (the heat conduction performance reaches 2.2W/mK) and the wave transmission performance (the dielectric loss and the loss tangent of the ceramic are close to zero) of the YSZ ceramic, the coloring capacity and the toughness (the fracture toughness can reach 6.5MPa m at most) of the YSZ ceramic are enhanced 1/2 ) The application of the mobile phone backboard and the wearable mobile electronic equipment is expanded.
6. The application value and the potential of SiC related materials in the civil market are greatly expanded.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the polycarbosilane solution with the mass percent of 10-20% in the first step is prepared by the following steps: polycarbosilane is weighed and dissolved in toluene. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: y in the yttria-stabilized zirconia described in step one 2 O 3 The mole percentage of (A) is 1.5% -8%. The rest is the same as the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the particle size of the yttria-stabilized zirconia is 50 nm-200 nm. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the dispersant in the first step is one or a mixture of several of sodium hexametaphosphate, cetyl trimethyl ammonium bromide and ammonium polyacrylate. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the cross-linking agent in the step one is one or a mixture of several of polyvinyl alcohol, polyethylene glycol and paraffin. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the sintering aid in the step one is copper oxide, aluminum oxide and Cu (NO) 3 ) 2 、Al(NO 3 ) 3 、Cu(OH) 2 And Al (OH) 3 One or a mixture of several of them. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the mixing in the step one is one or more of ball milling, sanding and high-speed shearing dispersion grinding; the dispersion medium adopted by mixing is one or a mixture of more of absolute ethyl alcohol, deionized water, cyclohexane and cyclopentane. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: in the first step, 98-99.6 parts of yttria-stabilized zirconia, 10-20 parts of polycarbosilane solution with the mass percent of 10% -20%, 0.1-0.5 part of sintering aid, 1-2 parts of dispersant and 1-1.5 parts of cross-linking agent are weighed and mixed according to the parts by mass. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: the compression molding in the step three is gel injection molding; the sintering in the third step is pressureless sintering, hot-pressing sintering, spark plasma sintering or microwave sintering; the atmosphere adopted by the sintering in the third step is vacuum, ar or Ar/H 2 And (4) mixing the gases. The others are the same as in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of zirconia ceramics for efficiently absorbing power frequency electromagnetic fields comprises the following steps:
1. weighing and mixing 98 parts by mass of yttria-stabilized zirconia, 10 parts by mass of 20% polycarbosilane solution, 0.1 part by mass of sintering aid, 1 part by mass of dispersant and 1 part by mass of cross-linking agent to obtain uniformly mixed slurry;
2. drying the uniformly mixed slurry at the temperature of 120 ℃ to obtain a dried mixed blank;
3. crushing and sieving the dried mixed blank to obtain powder with the grain size of 10-20 microns, and performing compression molding and sintering on the powder with the grain size of 10-20 microns to obtain the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field.
The polycarbosilane solution with the mass percent of 20% in the first step is prepared by the following steps: polycarbosilane is weighed and dissolved in toluene.
The yttria-stabilized zirconia in the first step is Y in Shandong province wear-resistant material Co., ltd (VK-R30) 2 O 3 Is 3%; the average grain diameter of the yttria-stabilized zirconia is 50nm; abbreviated as 3YSZ.
The dispersant in the first step is sodium hexametaphosphate.
The cross-linking agent in the first step is polyvinyl alcohol.
The sintering aid in the step one is alumina.
The mixing in the step one is ball milling, and the method specifically comprises the following steps: mixing the powder and a dispersion medium, and carrying out ball milling for 12 hours at the rotating speed of 300 r/min; the dispersion medium adopted by mixing is deionized water.
The compression molding in the third step is gel injection molding, and particularly, the pressure is maintained for 5min under the condition that the pressure is 20 MPa;
the sintering in the third step is pressureless sintering, which is specifically carried out according to the following steps: pre-burning for 4h at 700 ℃ in an air atmosphere to remove various additives to obtain a pre-burned blank, putting the pre-burned blank into a tube furnace, and sintering for 2h at 1500 ℃ in an argon atmosphere.
Through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by the pyrolyzed polycarbosilane to yttria-stabilized zirconia is 0.25 to 99.75, namely the content of the SiC powder is 0.25vol%.
The second embodiment: the difference between the present embodiment and the first embodiment is: in the first step, the addition amount of 20% polycarbosilane solution by mass is changed, and through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by pyrolysis of polycarbosilane to yttria-stabilized zirconia is 0.5. The rest is the same as the first embodiment.
Example three: the difference between the present embodiment and the first embodiment is: in the first step, the addition amount of 20% polycarbosilane solution by mass is changed, and through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by pyrolysis of polycarbosilane to yttria-stabilized zirconia is 1. The rest is the same as in the first embodiment.
Example four: the difference between the present embodiment and the first embodiment is: in the first step, the addition amount of 20% polycarbosilane solution by mass is changed, and through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by pyrolysis of polycarbosilane to yttria-stabilized zirconia is 3. The rest is the same as the first embodiment.
Example five: the difference between the present embodiment and the first embodiment is: in the first step, the addition amount of 20% polycarbosilane solution by mass is changed, and through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by pyrolysis of polycarbosilane to yttria-stabilized zirconia is 5. The rest is the same as the first embodiment.
Example six: the difference between the present embodiment and the first embodiment is: in the first step, the addition amount of 20% polycarbosilane solution by mass is changed, and through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by pyrolysis of polycarbosilane to yttria-stabilized zirconia is 10. The rest is the same as in the first embodiment.
Example seven: the difference between the present embodiment and the first embodiment is: in the first step, the addition amount of 20% polycarbosilane solution by mass is changed, and through calculation, in the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field, the volume ratio of SiC powder generated by pyrolysis of polycarbosilane to yttria-stabilized zirconia is 20. The rest is the same as the first embodiment.
Comparative experiment: the difference between this comparative experiment and the first example is that: the addition of a polycarbosilane solution with a mass percent of 20% is eliminated. The rest is the same as the first embodiment.
FIG. 1 is an element distribution diagram, wherein a is powder with a particle size of 10 μm to 20 μm prepared in step three of the example, and b is a section of the zirconia ceramic with high efficiency of absorbing the power frequency electromagnetic field prepared in the example one; as can be seen, siC was uniformly distributed in the system before and after sintering.
FIG. 2 is an XRD spectrum of zirconia ceramics with different SiC contents and high-efficiency absorption of power frequency electromagnetic field, and 1 is trueExample one, 2 is example two, 3 is example three, 4 is example four, 5 is example five, 6 is example six, 7 is example seven, 8 is 3YSZ,. Diamond-solid. Is t-ZrO 2 96795 is m-ZrO 2 ，
Is beta-SiC; as can be seen from the graph, XRD did not show a SiC peak at a low content, a SiC peak appeared at a high content, and stress was caused by mismatch of thermal expansion coefficients of SiC and 3YSZ at a high content, resulting in m-ZrO 2 And the composite ceramic added with SiC has weak SiC characteristic peak compared with pure YSZ ceramic.
Testing the hardness and the bending strength according to GB/T3297-1982 and GB/T39826-2021 standards, wherein fig. 3 is a comparison graph of the hardness and the bending strength of the zirconium oxide ceramics with different SiC contents and high-efficiency power frequency electromagnetic field absorption, a is the hardness, and b is the bending strength; as can be seen from the figure, the addition of a small amount of SiC does not obviously affect the hardness and the bending strength of the ceramic, the hardness can be more than 13GPa and can reach 13.35GPa at most, the bending strength is more than 300MPa and can reach 350MPa at most.
Testing the fracture toughness according to the GB/T14389-1993 standard, wherein a graph 4 shows a fracture toughness comparison graph of the zirconium oxide ceramics with different SiC contents and high-efficiency power frequency electromagnetic field absorption; as can be seen from the figure, the addition of a small amount of SiC can also effectively improve the fracture toughness of the zirconia ceramic, and the maximum fracture toughness can reach 6.5MPa m 1/2 。
Testing the wave absorbing performance according to SJ 20155-1992 standard, wherein FIG. 5 is a wave absorbing performance diagram of the zirconia ceramic which is prepared in the fifth embodiment and efficiently absorbs the power frequency electromagnetic field; indicating that lower SiC content does not affect ZrO 2 The wave-transparent performance of the ceramic, the dielectric loss and the loss tangent of the ceramic are close to zero.
Testing the heat conduction performance according to the GBT 39862-2021 standard, wherein FIG. 6 is a comparison graph of the heat conduction performance of the zirconium oxide ceramics with different SiC contents and high efficiency of absorbing the power frequency electromagnetic field; the heat-conducting property of the dual-phase ceramic is increased and then reduced along with the addition of SiC, which shows that the heat-conducting capability of the mobile phone back plate can be improved by adding the low-content SiC, the heat-conducting capability can be reduced due to the reduction of compactness by adding the low-content SiC excessively, and the heat-conducting property of the zirconia ceramic is improved from 1.8W/mK to 2.2W/mK by injecting the SiC.
FIG. 7 is a diagram of a zirconium oxide ceramic capable of efficiently absorbing a power frequency electromagnetic field prepared in example III and example V, wherein a is example III, and b is example V; the inset is a sintered black zirconia ceramic, and it can be seen that a deep, pure black zirconia ceramic can be obtained with a small amount of SiC added.
Claims (4)
1. The preparation method of the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field is characterized by comprising the following steps of:
1. weighing and mixing 95-99.6 parts by mass of yttria-stabilized zirconia, 1-20 parts by mass of 10-20% polycarbosilane solution, 0.1-0.5 part by mass of sintering aid, 0.2-2 parts by mass of dispersant and 0.3-1.5 parts by mass of cross-linking agent to obtain uniformly mixed slurry;
y in the yttria-stabilized zirconia 2 O 3 Is 3%; the average grain diameter of the yttria-stabilized zirconia is 50nm; the dispersant is sodium hexametaphosphate; the cross-linking agent is polyvinyl alcohol; the sintering aid is aluminum oxide;
2. drying the uniformly mixed slurry at the temperature of 100-140 ℃ to obtain a dried mixed blank;
3. crushing and sieving the dried mixed blank to obtain powder with the particle size of 10-20 microns, and performing compression molding and sintering on the powder with the particle size of 10-20 microns to obtain the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field;
the pyrolytic polycarbosilane generates SiC powder, and the SiC powder can efficiently absorb a power frequency electromagnetic field in the zirconia ceramic, wherein the SiC powder accounts for 0.25-1 vol% of the total volume of the SiC powder and yttria-stabilized zirconia;
the sintering is pressureless sintering, and specifically comprises the following steps: pre-burning for 4h at 700 ℃ in an air atmosphere to remove various additives to obtain a pre-burned blank, putting the pre-burned blank into a tube furnace, and sintering for 2h at 1500 ℃ in an argon atmosphere.
2. The preparation method of the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field according to claim 1, wherein the polycarbosilane solution with the mass percentage of 10% -20% in the first step is prepared by the following steps: polycarbosilane is weighed and dissolved in toluene.
3. The preparation method of the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field according to claim 1, wherein the mixing in the step one is one or more of ball milling, sand milling and high-speed shearing dispersion grinding; the dispersion medium adopted by mixing is one or a mixture of more of absolute ethyl alcohol, deionized water, cyclohexane and cyclopentane.
4. The preparation method of the zirconia ceramic capable of efficiently absorbing the power frequency electromagnetic field according to claim 1, characterized in that in the first step, 98-99.6 parts by mass of yttria-stabilized zirconia, 10-20 parts by mass of 10-20% polycarbosilane solution, 0.1-0.5 part by mass of sintering aid, 1-2 parts by mass of dispersant and 1-1.5 parts by mass of cross-linking agent are weighed and mixed.
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