CN108975763B - Preparation method of molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate - Google Patents
Preparation method of molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate Download PDFInfo
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- CN108975763B CN108975763B CN201810919936.2A CN201810919936A CN108975763B CN 108975763 B CN108975763 B CN 108975763B CN 201810919936 A CN201810919936 A CN 201810919936A CN 108975763 B CN108975763 B CN 108975763B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 197
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910021344 molybdenum silicide Inorganic materials 0.000 title claims abstract description 83
- 239000000919 ceramic Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 27
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 239000005011 phenolic resin Substances 0.000 claims abstract description 25
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 25
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 238000001291 vacuum drying Methods 0.000 claims abstract description 18
- 238000000465 moulding Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 17
- 238000002425 crystallisation Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- 239000000049 pigment Substances 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 5
- 239000007769 metal material Substances 0.000 description 3
- 238000010345 tape casting Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/12—Condensation polymers of aldehydes or ketones
- C04B26/122—Phenol-formaldehyde condensation polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
- C04B18/023—Fired or melted materials
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04M—TELEPHONIC COMMUNICATION
- H04M1/00—Substation equipment, e.g. for use by subscribers
- H04M1/02—Constructional features of telephone sets
- H04M1/0202—Portable telephone sets, e.g. cordless phones, mobile phones or bar type handsets
- H04M1/0279—Improving the user comfort or ergonomics
- H04M1/0283—Improving the user comfort or ergonomics for providing a decorative aspect, e.g. customization of casings, exchangeable faceplate
-
- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04M—TELEPHONIC COMMUNICATION
- H04M1/00—Substation equipment, e.g. for use by subscribers
- H04M1/02—Constructional features of telephone sets
- H04M1/18—Telephone sets specially adapted for use in ships, mines, or other places exposed to adverse environment
- H04M1/185—Improving the rigidity of the casing or resistance to shocks
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Civil Engineering (AREA)
- Signal Processing (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate, which comprises the steps of dispersing and adding 12-18 parts by weight of molybdenum silicide whiskers into isopropanol, and stirring to obtain a suspension A; adding 100 parts by weight of zirconia raw material into the suspension A successively, and stirring to obtain a suspension B; transferring the suspension B into a vacuum drying oven for vacuum drying to obtain powdery molybdenum silicide whisker/zirconia precursor; transferring the powdery molybdenum silicide whisker/zirconia precursor to an atmosphere furnace to sinter into molybdenum silicide whisker toughened zirconia ceramic powder; adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder, mixing uniformly, injecting the mixture into a mobile phone backboard mold, and performing hot press molding to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone backboard. The preparation method of the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate is simple and easy to operate, is beneficial to large-scale mass production, and improves the property and market competitiveness of the product.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone backboard.
Background
With the continuous development and technology updating of the mobile phone manufacturing industry, the demetalization of the mobile phone appearance is a trend, and non-metal materials such as glass appearance accessories and ceramic appearance accessories gradually replace metal material mobile phone appearance accessories, so that the mobile phone has strong market competitiveness.
The appearance of the ceramic mobile phone is excellent, is popular with mobile phone manufacturers, and is limited by cost and capacity at present. Compared with other materials, the ceramic mobile phone appearance accessory has higher hardness, can not be scratched, has excellent texture, is as warm as jade, and does not have the problem of signal shielding of metal materials. The ceramic mobile phone appearance accessories are mostly made of structural ceramics in special ceramics. Because of the property of phase change toughening, the structural ceramic mostly adopts zirconia ceramic. The zirconia ceramics have the excellent properties of high melting point, high hardness, scratch resistance and the like. Pure zirconia is white and appears when containing impuritiesYellow or gray, generally containing HfO2And is not easy to separate. However, zirconia ceramics also have the problems of poor toughness and easy cracking.
Chinese patent CN201711366286.5 discloses a method for manufacturing a zirconia ceramic mobile phone rear cover by using a tape casting process, which comprises the steps of ball-milling a zirconia ceramic powder raw material for manufacturing the zirconia ceramic mobile phone rear cover, mixing and stirring the raw material and an additive together, then carrying out secondary wet grinding to obtain a premixed slurry, mixing the premixed slurry and an organic plasticizer solution to prepare a mixed slurry with a certain viscosity, carrying out tertiary grinding on the mixed slurry to obtain a tape casting slurry, and carrying out vacuum defoaming treatment on the tape casting slurry; then the casting slurry flows into a zirconia ceramic mobile phone rear cover die from a container, and is coated on the zirconia ceramic mobile phone rear cover die in a scraping way according to the thickness of the zirconia ceramic mobile phone rear cover by a scraper, and the zirconia ceramic mobile phone rear cover die is peeled from the upper part after being dried and cured to form a rear cover green body, and then the green body is subjected to punching and laminating processing according to the size and the shape of the zirconia ceramic mobile phone rear cover to be made into a blank; sintering to obtain a zirconia ceramic mobile phone rear cover blank; and processing to obtain a zirconia ceramic mobile phone rear cover finished product. However, the zirconia ceramic mobile phone rear cover prepared by the patent does not modify zirconia, and still has the problems of poor toughness and easy fracture of the mobile phone rear cover.
Therefore, in order to solve the above problems, it is necessary to provide a method for preparing a toughened and modified zirconia ceramic mobile phone back plate, which improves the product properties and market competitiveness of the external fittings of the ceramic mobile phone.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate.
The technical scheme adopted by the invention for solving the problems is as follows: a preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
s1, dispersing and adding 12-18 parts by weight of molybdenum silicide whiskers into isopropanol, and stirring at a rotating speed of 300-400 r/min for 4-6 h to obtain a suspension A;
step S2, adding 100 parts by weight of zirconia raw material into the suspension A obtained in the step S1 one by one, and stirring at a rotating speed of 250 r/min-300 r/min for 4-8 h to obtain a suspension B;
step S3, transferring the suspension B obtained in the step S2 to a vacuum drying oven for vacuum drying for 8-12 h to obtain powdery molybdenum silicide whisker/zirconia precursor;
step S4, transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step S3 to a tubular vacuum atmosphere furnace to sinter into molybdenum silicide whisker toughened zirconia ceramic powder;
and S5, adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step S4, uniformly mixing, injecting into a mobile phone backboard mold, and performing hot press molding to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone backboard.
Further, in step S1, the ratio of the addition amount of isopropanol to the mass of molybdenum silicide whiskers is: 12-18 g of 1L.
Further, in step S4, the sintering process in the tubular vacuum atmosphere furnace includes a slow temperature rising process, a heat preservation crystallization process, a fast temperature lowering process, and a secondary cooling process.
Further, the slow temperature rise process specifically includes: slowly heating to 1300-1350 ℃ at a heating rate of 2-5 ℃.
Furthermore, the heat preservation crystallization process specifically comprises the following steps: and (3) carrying out heat preservation crystallization for 1.5-3 h at the temperature of 1300-1350 ℃.
Furthermore, the rapid cooling process specifically comprises: and cooling to 650-700 ℃ at a cooling rate of 60-80 ℃.
Further, the secondary cooling process specifically comprises: and naturally cooling to room temperature from 650 ℃ to 700 ℃.
Furthermore, in the step S5, the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.5-1 ml:10 g.
Further, in step S5, the hot press forming specifically includes: the forming temperature is 100-120 ℃, and the pressure maintaining pressure is 1.2-2.5 MPa.
Further, step S5 includes a step of adding various pigments into the liquid phenolic resin to adjust the color of the mobile phone back panel.
The invention has the advantages that:
1. according to the invention, the molybdenum silicide whisker toughened zirconia is used as a raw material to prepare the ceramic mobile phone back plate, so that the toughness and the shock resistance of the ceramic mobile phone back plate are improved; the molybdenum silicide whisker has the advantages of high temperature resistance, good toughness and metallic luster, toughens zirconia, improves the toughness and the shock resistance of the zirconia, improves the product performance of the ceramic mobile phone back plate, and improves the product glossiness of the ceramic mobile phone back plate;
2. the preparation method of the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate is simple and easy to operate, is beneficial to large-scale mass production, and improves the property and market competitiveness of the product.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
Example 1
A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
(1) dispersing 120g of molybdenum silicide whiskers into 10L of isopropanol, and stirring for 4 hours at the rotating speed of 300r/min to obtain a suspension A;
(2) successively adding 1000g of zirconia raw material into the suspension A obtained in the step S1, and stirring for 4 hours at the rotating speed of 250r/min to obtain a suspension B;
(3) transferring the suspension B obtained in the step (2) into a vacuum drying oven with the temperature of 80 ℃ for vacuum drying for 8h to obtain powdery molybdenum silicide whisker/zirconia precursor;
(4) transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step (3) to a tubular vacuum atmosphere furnace, slowly heating to 1300 ℃ at a heating rate of 2 ℃ per minute, carrying out heat preservation and crystallization for 1.5h at a temperature condition of 1300 ℃, then cooling to 650 ℃ at a cooling rate of 60 ℃ per minute, and naturally cooling to room temperature from 650 ℃ to form molybdenum silicide whisker toughened zirconia ceramic powder;
(5) adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step (4), adding titanium dioxide pigment into the liquid phenolic resin to adjust the color of the mobile phone back plate, uniformly mixing, injecting the mixture into a mobile phone back plate mold, and performing hot press molding under the conditions that the molding temperature is 100 ℃ and the pressure maintaining pressure is 1.2MPa to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate; wherein the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.5ml to 10 g.
Example 2
A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
(1) dispersing 180g of molybdenum silicide whiskers into 10L of isopropanol, and stirring for 6 hours at the rotating speed of 400r/min to obtain a suspension A;
(2) successively adding 1000g of zirconia raw material into the suspension A obtained in the step S1, and stirring for 8 hours at the rotating speed of 300r/min to obtain a suspension B;
(3) transferring the suspension B obtained in the step (2) into a vacuum drying oven with the temperature of 90 ℃ for vacuum drying for 12 hours to obtain powdery molybdenum silicide whisker/zirconia precursor;
(4) transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step (3) to a tubular vacuum atmosphere furnace, slowly heating to 1350 ℃ at a heating rate of 5 ℃ per minute, carrying out heat preservation and crystallization for 3h under the temperature condition of 1350 ℃, then cooling to 700 ℃ at a cooling rate of 80 ℃ per minute, and naturally cooling to room temperature from 700 ℃ to obtain molybdenum silicide whisker toughened zirconia ceramic powder;
(5) adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step (4), adding a lead-chromium yellow pigment into the liquid phenolic resin to adjust the color of the mobile phone back plate, uniformly mixing, injecting the mixture into a mobile phone back plate mold, and performing hot press molding under the conditions that the molding temperature is 120 ℃ and the pressure maintaining pressure is 2.5MPa to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate; wherein the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 1ml to 10 g.
Example 3
A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
(1) dispersing 150g of molybdenum silicide whiskers into 10L of isopropanol, and stirring for 5 hours at the rotating speed of 350r/min to obtain a suspension A;
(2) successively adding 1000g of zirconia raw material into the suspension A obtained in the step S1, and stirring for 6 hours at the rotating speed of 275r/min to obtain a suspension B;
(3) transferring the suspension B obtained in the step (2) to a vacuum drying oven for vacuum drying for 10 hours to obtain powdery molybdenum silicide whisker/zirconia precursor;
(4) transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step (3) to a tubular vacuum atmosphere furnace, slowly heating to 1325 ℃ at the heating rate of 3.5 ℃ per minute, carrying out heat preservation and crystallization for 2.2h at the temperature of 1325 ℃, then cooling to 675 ℃ at the cooling rate of 70 ℃ per minute, and naturally cooling to room temperature from 675 ℃, thereby forming molybdenum silicide whisker toughened zirconia ceramic powder;
(5) adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step (4), adding various pigments into the liquid phenolic resin to adjust the color of the mobile phone back plate, uniformly mixing, injecting the mixture into a mobile phone back plate mold, and performing hot press molding under the conditions that the molding temperature is 110 ℃ and the pressure maintaining pressure is 1.8MPa to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate; wherein the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.75ml to 10 g.
Example 4
A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
(1) dispersing 130g of molybdenum silicide whiskers into 10L of isopropanol, and stirring for 4.5h at the rotating speed of 320r/min to obtain a suspension A;
(2) successively adding 1000g of zirconia raw material into the suspension A obtained in the step S1, and stirring for 5 hours at the rotating speed of 260r/min to obtain a suspension B;
(3) transferring the suspension B obtained in the step (2) to a vacuum drying oven for vacuum drying for 9 hours to obtain powdery molybdenum silicide whisker/zirconia precursor;
(4) transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step (3) into a tubular vacuum atmosphere furnace, slowly heating to 1310 ℃ at a heating rate of 3 ℃ per minute, carrying out heat preservation and crystallization for 2 hours at a temperature condition of 1310 ℃, then cooling to 660 ℃ at a cooling rate of 65 ℃ per minute, and naturally cooling to room temperature from 660 ℃ to form molybdenum silicide whisker toughened zirconia ceramic powder;
(5) adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step (4), adding various pigments into the liquid phenolic resin to adjust the color of the mobile phone back plate, uniformly mixing, injecting the mixture into a mobile phone back plate mold, and performing hot press molding under the conditions that the molding temperature is 105 ℃ and the pressure maintaining pressure is 1.5MPa to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate; wherein the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.6ml to 10 g.
Example 5
A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
(1) dispersing 170g of molybdenum silicide whiskers into 10L of isopropanol, and stirring for 5.5 hours at the rotating speed of 380r/min to obtain a suspension A;
(2) successively adding 100 parts by weight of zirconia raw material into the suspension A obtained in the step S1, and stirring for 7 hours at the rotating speed of 290r/min to obtain a suspension B;
(3) transferring the suspension B obtained in the step (2) to a vacuum drying oven for vacuum drying for 11h to obtain powdery molybdenum silicide whisker/zirconia precursor;
(4) transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step (3) to a tubular vacuum atmosphere furnace, slowly heating to 1340 ℃ at a heating rate of 4.5 ℃ per minute, carrying out heat preservation crystallization for 2.5 hours at a temperature of 1340 ℃, then cooling to 690 ℃ at a cooling rate of 75 ℃ per minute, and naturally cooling to room temperature from 690 ℃, thereby forming molybdenum silicide whisker toughened zirconia ceramic powder;
(5) adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step (4), adding various pigments into the liquid phenolic resin to adjust the color of the mobile phone back plate, uniformly mixing, injecting the mixture into a mobile phone back plate mold, and performing hot press molding under the conditions that the molding temperature is 115 ℃ and the pressure maintaining pressure is 2.2MPa to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate; wherein the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.9ml to 10 g.
Example 6
A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate comprises the following steps:
(1) dispersing 175g of molybdenum silicide whiskers into 10L of isopropanol, and stirring for 5 hours at the rotating speed of 310r/min to obtain a suspension A;
(2) successively adding 1000g of zirconia raw material into the suspension A obtained in the step S1, and stirring for 6.5 hours at the rotating speed of 280r/min to obtain a suspension B;
(3) transferring the suspension B obtained in the step (2) to a vacuum drying oven for vacuum drying for 10 hours to obtain powdery molybdenum silicide whisker/zirconia precursor;
(4) transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step (3) to a tubular vacuum atmosphere furnace, slowly heating to 1330 ℃ at a heating rate of 3 ℃/min, carrying out heat preservation and crystallization for 2h at 1330 ℃ and then cooling to 680 ℃ at a cooling rate of 75 ℃/min, and naturally cooling to room temperature from 680 ℃ to form molybdenum silicide whisker toughened zirconia ceramic powder;
(5) adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step (4), adding various pigments into the liquid phenolic resin to adjust the color of the mobile phone back plate, uniformly mixing, injecting the mixture into a mobile phone back plate mold, and performing hot press molding under the conditions that the molding temperature is 112 ℃ and the pressure maintaining pressure is 2.4MPa to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate; wherein the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.8ml to 10 g.
Experimental example 1
The molybdenum silicide whisker toughened zirconia ceramic mobile phone back plates prepared by the preparation methods of the embodiments 1 to 6 are marked as Y1 to Y6, and the performance of Y1 to Y6 is tested, and the test results are shown in Table 1.
Table 1 performance test results of the molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate prepared by the preparation methods of examples 1 to 6
Item | Fracture toughness | Mohs hardness | Vickers hardness | Flexural strength | Thermal conductivity |
Y1 | 27MPa·m1/2 | 9 | 1360HV | 1350MPa | 2W/mK |
Y2 | 28MPa·m1/2 | 9.2 | 1380HV | 1380MPa | 1.8W/mK |
Y3 | 29MPa·m1/2 | 9.3 | 1400HV | 1400MPa | 1.7W/mK |
Y4 | 28.5MPa·m1/2 | 9.5 | 1410HV | 1390MPa | 1.9W/mK |
Y5 | 27.5MPa·m1/2 | 9.3 | 1390HV | 1380MPa | 1.8W/mK |
Y6 | 27.2MPa·m1/2 | 9.1 | 1365HV | 1370MPa | 1.92W/mK |
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of a molybdenum silicide whisker toughened zirconia ceramic mobile phone back plate is characterized by comprising the following steps:
step S1, dispersing and adding 12-18 parts by weight of molybdenum silicide whiskers into isopropanol, and stirring for 4-6 h at the rotating speed of 300-400 r/min to obtain suspension A;
step S2, adding 100 parts by weight of zirconia raw material into the suspension A obtained in the step S1 one by one, and stirring at the rotating speed of 250 r/min-300 r/min for 4 h-8 h to obtain a suspension B;
step S3, transferring the suspension B obtained in the step S2 to a vacuum drying oven for vacuum drying for 8-12 h to obtain powdery molybdenum silicide whisker/zirconia precursor;
step S4, transferring the powdery molybdenum silicide whisker/zirconia precursor obtained in the step S3 to a tubular vacuum atmosphere furnace to sinter into molybdenum silicide whisker toughened zirconia ceramic powder;
step S5, adding liquid phenolic resin into the molybdenum silicide whisker toughened zirconia ceramic powder obtained in the step S4, uniformly mixing, injecting the mixture into a mobile phone backboard mold, and performing hot press molding to obtain the molybdenum silicide whisker toughened zirconia ceramic mobile phone backboard;
in step S4, the sintering process of the tubular vacuum atmosphere furnace includes a slow temperature rise process, a heat preservation crystallization process, a rapid temperature reduction process, and a secondary cooling process;
the slow heating process specifically comprises the following steps: slowly heating to 1300-1350 ℃ at the heating rate of 2-5 ℃/min;
the heat-preservation crystallization process specifically comprises the following steps: keeping the temperature and crystallizing for 1.5 to 3 hours at the temperature of 1300 to 1350 ℃;
the rapid cooling process specifically comprises the following steps: cooling to 650-700 ℃ at a cooling rate of 60-80 ℃/min;
the secondary cooling process specifically comprises the following steps: naturally cooling to room temperature from 650-700 ℃.
2. The preparation method according to claim 1, wherein in step S1, the ratio of the addition amount of isopropanol to the mass of molybdenum silicide whiskers is: 12g to 18g for 1L.
3. The preparation method according to claim 1, wherein in step S5, the ratio of the addition amount of the liquid phenolic resin to the weight of the molybdenum silicide whisker toughened zirconia ceramic powder is 0.5-1 ml:10 g.
4. The method according to claim 1, wherein in step S5, the hot press forming is specifically: the molding temperature is 100-120 ℃, and the pressure maintaining pressure is 1.2-2.5 MPa.
5. The method for preparing the mobile phone back plate according to claim 1, wherein the step S5 further comprises the step of adding various pigments into the liquid phenolic resin to adjust the color of the mobile phone back plate.
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