CN107417296B - Honeycomb blind hole toughened zirconia ceramic mobile phone back plate and preparation method thereof - Google Patents
Honeycomb blind hole toughened zirconia ceramic mobile phone back plate and preparation method thereof Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 101
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- 239000007788 liquid Substances 0.000 claims description 8
- JPNZKPRONVOMLL-UHFFFAOYSA-N azane;octadecanoic acid Chemical compound [NH4+].CCCCCCCCCCCCCCCCCC([O-])=O JPNZKPRONVOMLL-UHFFFAOYSA-N 0.000 claims description 7
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 7
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- 238000005299 abrasion Methods 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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- 239000007858 starting material Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical group [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
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- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/48—Macromolecular compounds
- C04B41/4853—Epoxides
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/4922—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as monomers, i.e. as organosilanes RnSiX4-n, e.g. alkyltrialkoxysilane, dialkyldialkoxysilane
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
- C04B41/83—Macromolecular compounds
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- 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
Abstract
The invention discloses a honeycomb blind hole toughened zirconia ceramic mobile phone back plate and a preparation method thereof, the process method comprises the steps of injection molding a mobile phone back plate biscuit, shaping the back plate at low temperature by utilizing the plasticity of the biscuit to obtain the mobile phone back plate biscuit with the honeycomb blind holes, injecting an organic polymer plastic material into the blind holes of a ceramic blank body and curing the biscuit after degreasing and sintering, organically combining the ceramic back plate with the organic polymer plastic material, wherein the organic polymer plastic material can effectively absorb impact energy in the collision and dropping process, the fracture toughness of the mobile phone back plate is improved, meanwhile, the organic polymer plastic material is hidden in the mobile phone ceramic back plate, the outer surface is an integral ceramic material, the appearance is attractive and elegant, meanwhile, the hard outer surface ceramic provides good wear resistance, and on the other hand, the density of the organic polymer plastic material is far lower than that of zirconia ceramic, the mobile phone back plate is light and thin.
Description
Technical Field
The invention relates to the field of structural member preparation, in particular to the field of consumer electronic backboard structural member preparation, and particularly relates to a honeycomb blind hole toughened zirconia ceramic mobile phone backboard and a preparation method thereof.
Background
With the rapid development of consumer electronics such as mobile phones, structural members such as housings (back panels) of consumer electronics have made great progress and new problems are encountered. Especially, the future 5G era puts more severe requirements on the material of the consumer electronics housing (back panel). Traditional metal brings huge challenge to antenna design due to its shielding effect, and it will not be used for the manufacturing of 5G shell (backplate), and its application in large size screen, ultra-thin field has been restricted to its innate low intensity, wearproof of plastics, and in addition along with the improvement of consumer aesthetics, traditional single metal shell and plastic material's shell (backplate) will also be difficult to the consumers of motivating.
Due to ZrO2Ceramics have high toughness, good hardness, high abrasion resistance, are widely applied in the fields of structural ceramics and functional ceramics, and it has been reported that partially stabilized zirconia (TZP) can be used for preparing corrosion-resistant watch cases, watches and other instrument parts by powder metallurgy. Therefore, in recent years, the application of the method to the mobile phone housing has been tried by researchers more and more. For example, in the patent with application number 201510309285.1, the main phase of zirconia is added with additives such as alumina and titania to prepare the mobile phone shell by casting. For example, in patent application No. 201510940002.3, a cell phone case is formed by mixing yttrium-stabilized zirconia ceramic powder with an organic material and extruding the mixture. In addition, according to the book of structural ceramics of Xie Shi Peng, the ZrO with best toughening performance in mass production is reported2The fracture toughness of the ceramic is only 8-12 MPa1/2Commercial use still has problems: zirconia ceramics still have poor fracture toughness and poor drop resistance compared to metals and plastics, which necessarily limits their applications. On the other hand, in order to achieve the same anti-falling performance of other materials, the zirconia ceramic backboard is inevitably made of ceramics with thicker size, the thickness of some ceramics exceeds 1mm, and the density of the zirconia ceramic reaches 6.1g/cm3This inevitably leads to the zirconia ceramic backplate being heavy, which is not consistent with the development route of electronic products being light and thin.
Disclosure of Invention
In view of the above, the present invention provides a cellular blind hole toughened zirconia ceramic mobile phone backplate, which is a zirconia ceramic mobile phone backplate, wherein the first plane of the backplate has more than one regular polygon blind holes, and organic polymer plastic material is cured and encapsulated in the blind holes.
Preferably, the organic polymer plastic material is epoxy resin or silica gel.
Preferably, the depth of the positive polygonal blind holes is 0.1-0.9 mm, the side length of a regular polygon of the regular polygonal blind holes is 0.5-10 mm, and the wall thickness of two adjacent regular polygonal blind holes is 0.5-3 mm.
Preferably, the regular polygon blind hole is one of an equilateral triangle blind hole, a square blind hole, a regular pentagon blind hole, a regular hexagon blind hole and a round blind hole.
In order to achieve the above object, in another aspect, the present invention provides a method for preparing a back plate of a mobile phone, which comprises the following steps:
a) carrying out high-temperature negative pressure banburying on a surface modifier, inorganic nano zirconia powder, paraffin and an organic high polymer material in a banbury mixer to obtain a feed;
b) injecting the molten feed into a mold with more than one regular polygon boss under the negative pressure of a mold cavity, and performing secondary mold closing, pressurizing and shaping in a semi-molten state to obtain a back plate biscuit with more than one regular polygon blind hole;
c) degreasing, preserving heat and sintering the back plate biscuit to obtain a back plate blank;
d) treating the regular polygonal blind hole of the back plate blank by using a surface modifier;
e) injecting liquid epoxy resin or liquid silica gel into the regular polygon blind hole of the backboard blank treated in the step d), and curing at the temperature of 60-180 ℃ for 5-120 min.
Preferably, the backing plate blank treated in step f) is machined.
Preferably, the shaping temperature in the step c) is 90-120 ℃, the shaping pressure is 150-250 MPa, and the shaping time is 1 s-2 min;
preferably, the organic polymer in the step a) is one of polyethylene, polypropylene and polyphenylene sulfide; the mass percent of the surface modifier is 0.5-0.8%, the mass percent of the inorganic nano zirconia powder is 85.2-92.5%, the mass percent of the paraffin is 4-9%, and the mass percent of the organic polymer is 3-5%.
Preferably, the thickness of the biscuit of the back plate in the step b) is 0.3 mm-2 mm.
Preferably, the hole depth of the regular polygonal blind holes shaped in the step b) is 0.1-0.9 mm, the side length of a regular polygon of the regular polygonal blind holes is 0.5-10 mm, the wall thickness of two adjacent regular polygonal blind holes is 0.5-3 mm, and the regular polygonal blind holes are one of equilateral triangle blind holes, square blind holes, regular pentagon blind holes, regular hexagon blind holes and round blind holes.
Preferably, the surface modifier in steps a) and d) is one of stearic acid, ammonium stearate and a silane coupling agent.
Preferably, the silane coupling agent is one or a combination of two of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560) and gamma- (methacryloyloxy) propyltrimethoxysilane (KH 570).
Preferably, the inorganic nano-zirconia powder is yttrium-stabilized nano-zirconia, and the D50 is 30nm to 200 nm.
Preferably, the banburying temperature in the step a) is 120-150 ℃, the negative pressure is-0.05 MPa-0.08 MPa, and the banburying time is 1-4 h.
Preferably, the injection molding temperature in the step b) is 130-155 ℃, and the negative pressure is-0.07 MPa to-0.09 MPa.
Preferably, the sintering temperature in the step c) is 1300-1500 ℃, and the heat preservation time is 2-4 h.
The invention has the beneficial effects that: the invention discloses a honeycomb blind hole toughened zirconia ceramic mobile phone back plate and a preparation method thereof. Compared with direct injection molding, the process of reshaping after injection molding solves the problem that thin-wall parts with the thickness less than 0.2mm cannot be injected. Organic polymer plastic material falls the effectual absorption impact energy of process ability in the collision in the blind hole, improves the fracture toughness of cell-phone backplate, and organic polymer plastic material hides inside cell-phone ceramic backplate simultaneously, does not influence pleasing to the eye, and surface ceramic part provides the good wear resistance of backplate, and compound ceramic backplate has reduced the quantity of pottery on the one hand in addition, does benefit to the backplate frivolousization.
Drawings
FIG. 1 is a schematic diagram of a preparation method of a honeycomb blind hole toughened zirconia ceramic mobile phone back plate.
Fig. 2 is a schematic view of a cellular circular blind hole internal cured epoxy resin toughened zirconia ceramic mobile phone back plate.
Detailed Description
The invention is described in further detail below, wherein the starting materials and the equipment used are commercially available without particular requirement. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention.
The honeycomb blind hole toughened zirconia ceramic mobile phone back plate disclosed by the invention is formed by shaping a plurality of regular polygon blind holes on the inner surface of the zirconia ceramic mobile phone back plate, and curing and packaging an organic polymer plastic material in the blind holes. This blind hole may also be an irregular polygonal blind hole, preferably a regular polygonal blind hole in this example.
In this embodiment, the organic polymer plastic material is epoxy resin or silicone.
In the example, the hole depth of the positive polygonal blind hole is 0.1 mm-0.9 mm, the side length of the regular polygon of the regular polygonal blind hole is 0.5 mm-10 mm, and the wall thickness of two adjacent regular polygon blind holes is 0.5 mm-3 mm.
In this example, the regular polygonal blind hole is one of an equilateral triangular blind hole, a square blind hole, a regular pentagonal blind hole, a regular hexagonal blind hole, and a circular blind hole.
In order to prepare the honeycomb blind hole toughened zirconia ceramic mobile phone back plate, the invention provides a preparation method of a mobile phone back plate, which comprises the following steps:
a) and banburying the surface modifier, the inorganic nano zirconia powder, the paraffin and the organic high polymer material in a banbury mixer at high temperature and under negative pressure to obtain the feed. In this embodiment, the preferred organic polymer is one of polyethylene, polypropylene, and polyphenylene sulfide; the mass percent of the surface modifier is 0.5-0.8%, the mass percent of the inorganic nano zirconia powder is 85.2-92.5%, the mass percent of the paraffin is 4-9%, and the mass percent of the organic polymer is 3-5%. In this example, the preferred surface modifying agent is one or a combination of two of stearic acid, ammonium stearate, and a silane coupling agent, which is one or a combination of two of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560), and gamma- (methacryloyloxy) propyltrimethoxysilane (KH 570). In this example, the preferred inorganic nano zirconia powder is yttrium stabilized nano zirconia with a D50 of 30nm to 200 nm. In this example, the mixing temperature is preferably 120 ℃ to 150 ℃ and the negative pressure in the cavity during the mixing in the mixer is-0.05 MPa to-0.08 MPa according to the different preferred organic polymers and the different paraffin content, and the mixing time is 1h to 4 h.
b) And injecting the molten feed into a mold with more than one regular polygon boss under the negative pressure of a mold cavity, and performing secondary mold closing and pressure shaping in a semi-molten state to obtain a back plate biscuit with more than one regular polygon blind hole. In the example, the preferable injection molding temperature in the injection molding stage is 130-155 ℃, the negative pressure of the mold cavity of the mold before injection is-0.07 MPa-0.09 MPa, and the thickness of the biscuit of the zirconia ceramic mobile phone backboard after injection is 0.3-2 mm. In the embodiment, the injection molding of the back plate biscuit with the thickness less than 0.2mm is avoided, the injection molding difficulty is increased, and the yield is not high. The mold is closed again, pressurized and reshaped and reamed under the semi-molten state before the material is completely solidified after injection molding, so that the thickness of the thinnest part of the back plate biscuit is smaller than 0.2mm, and the problem that the back plate biscuit with the thickness smaller than 0.2mm cannot be directly injected is solved. In this embodiment for better shaping. Preferably, the temperature of the die in the shaping stage is 90-120 ℃, the shaping pressure is 150-250 MPa, and the shaping time is 1 s-2 min. In this example, the shaped regular polygonal blind hole is one of an equilateral triangular blind hole, a square blind hole, a regular pentagonal blind hole, a regular hexagonal blind hole, and a circular blind hole. In the example, the hole depth of the positive polygonal blind hole is 0.1 mm-0.9 mm, the side length of the regular polygon of the regular polygonal blind hole is 0.5 mm-10 mm, and the wall thickness of two adjacent regular polygon blind holes is 0.5 mm-3 mm.
c) Degreasing, heat-preserving and sintering the backboard biscuit processed in the step b) to obtain a backboard blank, wherein the preferable sintering temperature in the example is 1300-1500 ℃, the heat-preserving time is 2-4 h, and in order to improve the product yield, the degreasing rate, the sintering temperature rise rate and the temperature reduction rate are all relatively slow.
d) Injecting liquid epoxy resin or liquid silica gel into the regular polygonal blind holes of the back plate blank, and curing at 60-180 ℃ for 5-120 min to obtain the honeycomb blind hole toughened zirconia ceramic mobile phone back plate, wherein in order to improve the bonding strength of the organic polymer plastic material and the inner surface of the blind holes of the mobile phone back plate blank, the sintered mobile phone back plate blank with the blind holes is subjected to modification treatment by using stearic acid (ammonium) or a silane coupling agent.
e) And e), processing burrs and allowance of the back plate blank processed in the step e) by using CNC (computerized numerical control) processing equipment, and then performing ceramic polishing treatment to obtain the honeycomb blind hole toughened zirconia ceramic mobile phone back plate.
The following are specific examples of the present invention:
example 1
Weighing 1.85kg of 3Y-TZP ceramic powder with stearic acid 10g and D50 of 200nm, 80g (4%) of No. 58 paraffin and 60g of polyphenylene sulfide, adding the weighed organic matters into a 3L internal mixer, heating to 120 ℃ to melt the organic matters, then adding the ceramic powder into the internal mixer for internal mixing for 3 times, pumping the internal mixer to-0.08 MPa after the ceramic powder is added, and internally mixing for 1h at 150 ℃ to obtain a feed. And (3) loading the feed into a hopper of an injection molding machine, loading a triangular blind hole mold with the dimension of 10mm side length, the blind hole depth of 0.9mm and the wall thickness of 3mm into the injection molding machine, and pumping a mold cavity to-0.07 MPa, wherein the mold cavity of the mold is 2mm thick and is 5 inches in size. Setting the temperature of a charging basket of an injection molding machine to be 155 ℃, the injection pressure to be 150MPa for injection molding, and the temperature of the mold to be 120 ℃, injecting the molten feed into a mold cavity at a high speed, maintaining the pressure for 1s, raising the mold locking force of the mold to 200MPa, shaping and maintaining the pressure for 1min, and obtaining a regular triangle blind hole mobile phone backboard biscuit with the side length of 10mm, the blind hole depth of 0.9mm and the wall thickness of 3 mm.
The mobile phone backboard biscuit is stacked and placed in a degreasing furnace, the temperature is slowly increased to 170 ℃ at the speed of 0.2 ℃/min, the temperature is maintained for 20 hours, then the mobile phone backboard biscuit is cooled along with the furnace, the stack of the mobile phone backboard biscuit is placed in a sintering furnace, the temperature is increased to 450 ℃ at the speed of 1 ℃/min, the temperature is maintained for two hours, then the temperature is increased to 650 ℃ at the speed of 1 ℃/min, the temperature is increased to 1500 ℃ at the speed of 5 ℃/min, the temperature is maintained for 2 hours, the temperature is reduced to 950 ℃ at the speed of 5 ℃/.
Weighing 50g of gamma-aminopropyltriethoxysilane (KH550) and adding the gamma-aminopropyltriethoxysilane into a mixed solution of 2kg of deionized water and 2kg of ethanol, then putting a mobile phone back plate blank into the mixed solution for soaking for 2h, then putting the mobile phone back plate blank into an oven for drying, then coating liquid epoxy resin into blind holes, scraping off redundant liquid epoxy resin, curing the liquid epoxy resin in the oven for 120min at 60 ℃, then processing burrs and the balance of the back plate blank by using CNC (computerized numerical control) processing equipment, and then polishing the back plate to obtain the honeycomb blind hole toughened zirconia ceramic mobile phone back plate.
The samples for testing the bending strength by a three-point bending method and the fracture toughness by a single-side notched beam method require multiple sampling tests to obtain an average value, and the test result shows that the bending strength of the composite ceramic is 1067MPa, and the fracture toughness is 14.8MPa.m1/2The bending strength of the currently commercial Y-TZP is usually 800-1200 MPa and the fracture toughness is 8-12 MPa.m according to the introduction of structural ceramics1/2. Compared with the commercial Y-TZP ceramic, the fracture toughness is obviously improved, and the Y-TZP ceramic is more suitable for mobile phone shells (back plates).
Example 2
Weighing 1.704kg of 3Y-TZP ceramic powder with ammonium stearate 16g and D50 of 30nm, 180g of No. 56 paraffin and 100g of polyethylene, adding the weighed organic matters into a 3L internal mixer, heating to 120 ℃ to melt the organic matters, then adding the ceramic powder into the internal mixer for internal mixing for 3 times, pumping the internal mixer to-0.05 MPa after the ceramic powder is added, and internally mixing for 4 hours at 120 ℃ to obtain a feed. And (3) loading the feed into a hopper of an injection molding machine, loading a square blind hole mold with the dimension of 0.5mm in side length, 0.1mm in blind hole depth and 0.5mm in wall thickness into the injection molding machine, and pumping a mold cavity to-0.09 MPa, wherein the mold cavity is 0.3mm in thickness and 4 inches in size. Setting the temperature of a charging basket of an injection molding machine to be 130 ℃, the injection pressure to be 200MPa for injection molding, and the temperature of a mold to be 110 ℃, injecting the molten feed into a mold cavity at a high speed for pressure maintaining for 1.5s, and raising the mold locking force of the mold to 250MPa for shaping and pressure maintaining for 1s to obtain a square blind hole mobile phone backboard biscuit with the side length of 0.5mm, the blind hole depth of 0.1mm and the wall thickness of 0.5 mm.
Stacking the mobile phone backboard biscuit, putting the stack into a degreasing furnace, slowly heating to 170 ℃ at the speed of 0.2 ℃/min, preserving heat for 20h, cooling along with the furnace, stacking the mobile phone backboard biscuit, putting the stack into a sintering furnace, heating to 400 ℃ at the speed of 1 ℃/min, preserving heat for two hours, heating to 650 ℃ at the speed of 1 ℃/min, heating to 1300 ℃ at the speed of 5 ℃/min, preserving heat for 4h, cooling to 950 ℃ at the speed of 5 ℃/min, and cooling along with the furnace to obtain the mobile phone backboard blank.
Weighing 30g of gamma-aminopropyltriethoxysilane (KH550) and 20g of gamma-glycidoxypropyltrimethoxysilane (KH560) and adding into a mixed solution of 2kg of deionized water and 2kg of ethanol, then putting the mobile phone back plate blank into the mixed solution for soaking for 2h, putting the mobile phone back plate blank into an oven for drying, then coating liquid silica gel into blind holes, scraping off redundant liquid silica gel resin, curing for 5min at 180 ℃ in the oven, then processing burrs and the balance of the back plate blank by using CNC (computerized numerical control) processing equipment, and then grinding and polishing the back plate to obtain the honeycomb blind hole toughened zirconium oxide ceramic mobile phone back plate.
The samples for testing the bending strength by a three-point bending method and the fracture toughness by a single-side notched beam method require multiple sampling tests to obtain an average value, and the test result shows that the bending strength of the composite ceramic is 1132MPa, and the fracture toughness is 14.1MPa.m1/2。
Example 3
Weighing 16g of gamma- (methacryloyloxy) propyltrimethoxysilane, 180g of No. 58 paraffin and 100g of polypropylene as 3Y-TZP ceramic powder with D50 of 30nm, adding the weighed organic matters into a 3L internal mixer, heating to 130 ℃ to melt the organic matters, then adding the ceramic powder into the internal mixer for internal mixing for 3 times, pumping the internal mixer to-0.05 MPa after the ceramic powder is added, and internally mixing for 3 hours at 135 ℃ to obtain a feed. And (3) loading the feed into a hopper of an injection molding machine, loading a regular five-shaped blind hole mold with the dimension of 5mm side length, the blind hole depth of 0.1mm and the wall thickness of 2mm into the injection molding machine, and pumping a mold cavity to-0.08 MPa, wherein the mold cavity of the mold is 0.8mm thick and 5.5 inches in size. Setting the temperature of a charging basket of an injection molding machine to 145 ℃, the injection pressure to 180MPa for injection molding, and the temperature of the mold to 90 ℃, injecting the molten feed into the mold cavity at a high speed for 2s for pressure maintaining, and raising the mold locking force of the mold to 150MPa for shaping and pressure maintaining for 2min to obtain a regular pentagonal blind hole mobile phone backboard blank with the side length of 5mm, the blind hole depth of 0.1mm and the wall thickness of 2 mm.
Stacking the mobile phone back plate biscuit, putting the stack into a degreasing furnace, slowly heating to 170 ℃ at the speed of 0.2 ℃/min, preserving heat for 20h, cooling along with the furnace, stacking the mobile phone back plate biscuit, putting the stack into a sintering furnace, heating to 430 ℃ at the speed of 1 ℃/min, preserving heat for two hours, heating to 650 ℃ at the speed of 1 ℃/min, heating to 1350 ℃ at the speed of 5 ℃/min, preserving heat for 2h, cooling to 950 ℃ at the speed of 5 ℃/min, and cooling along with the furnace to obtain the mobile phone back plate blank.
Weighing 50g of gamma- (methacryloyloxy) propyl trimethoxy silane, adding the gamma- (methacryloyloxy) propyl trimethoxy silane into a mixed solution of 2kg of deionized water and 2kg of ethanol, putting a mobile phone back plate blank into the mixed solution, soaking for 2h, putting the mobile phone back plate blank into an oven, drying, coating liquid silica gel into blind holes, scraping off redundant liquid silica gel, curing for 10min at 180 ℃ in the oven, processing burrs and the balance of the back plate blank by using CNC (computerized numerical control) processing equipment, and polishing the ceramic back plate blank to obtain the honeycomb blind hole toughened zirconia ceramic mobile phone back plate.
The samples for testing the bending strength by a three-point bending method and the fracture toughness by a single-side notched beam method require multiple sampling tests to obtain an average value, and the test result shows that the bending strength of the composite ceramic is 1209MPa, and the fracture toughness is 15.6MPa1/2。
Example 4
Weighing 1.708kg of 8Ce-TZP ceramic powder with gamma-aminopropyltriethoxysilane 12g and D50 of 50nm, 180g of No. 58 paraffin and 100g of polypropylene, adding the weighed organic matters into a 3L internal mixer, heating to 130 ℃ to melt the organic matters, adding the ceramic powder into the internal mixer for 3 times, pumping the internal mixer to-0.07 MPa after the ceramic powder is added, and internally mixing for 3 hours at 140 ℃ to obtain a feed. And (3) loading the feed into a hopper of an injection molding machine, loading a regular hexagonal blind hole mold with the dimension of 3mm side length, the blind hole depth of 0.3mm and the wall thickness of 2mm into the injection molding machine, and pumping a mold cavity to-0.08 MPa, wherein the mold cavity of the mold is 1.2mm thick and 6 inches in size. Setting the temperature of a charging basket of an injection molding machine to be 150 ℃, the injection pressure to be 190MPa for injection molding, and the temperature of the mold to be 100 ℃, injecting the molten feed into a mold cavity at a high speed for maintaining the pressure for 1s, and then increasing the mold locking force to 220MPa for shaping and maintaining the pressure for 30s to obtain a regular hexagonal blind hole mobile phone back panel biscuit with the side length of 3mm, the blind hole depth of 0.3mm and the wall thickness of 2 mm.
Stacking the mobile phone backboard biscuit, putting the stack into a degreasing furnace, slowly heating to 170 ℃ at the speed of 0.2 ℃/min, preserving heat for 20h, cooling along with the furnace, stacking the mobile phone backboard biscuit, putting the stack into a sintering furnace, heating to 420 ℃ at the speed of 1 ℃/min, preserving heat for two hours, heating to 650 ℃ at the speed of 1 ℃/min, heating to 1400 ℃ at the speed of 5 ℃/min, preserving heat for 2h, cooling to 950 ℃ at the speed of 5 ℃/min, and cooling along with the furnace to obtain the mobile phone backboard blank.
Weighing 50g of stearic acid, adding the stearic acid into 3kg of ethanol solution, uniformly mixing, then putting the mobile phone back plate blank into the ethanol solution, soaking for 3h, putting the mobile phone back plate blank into an oven for drying, then coating liquid epoxy resin into the blind holes, scraping redundant liquid epoxy resin, curing for 40min at 80 ℃ in the oven, then processing burrs and the balance of the back plate blank by using CNC (computerized numerical control) processing equipment, and then performing ceramic grinding and polishing treatment to obtain the honeycomb blind hole toughened zirconia ceramic mobile phone back plate.
The samples for testing the bending strength by a three-point bending method and the fracture toughness by a single-side notched beam method require multiple sampling tests to obtain an average value, and the test result shows that the bending strength of the composite ceramic is 1104MPa, and the fracture toughness is 14.9MPa1/2。
Example 5
Weighing 6g of gamma-glycidoxypropyltrimethoxysilane, 6g of gamma- (methacryloyloxy) propyltrimethoxysilane, 1.708kg of 3Y-TZP ceramic powder with D50 of 30nm, 160g of No. 56 paraffin and 80g of polyphenylene sulfide, adding the weighed organic matters into a 3L internal mixer, heating to 145 ℃ for melting, adding the ceramic powder into the internal mixer for internal mixing for 3 times, pumping the internal mixer to negative pressure of-0.06 MPa after the ceramic powder is added, and internally mixing for 2 hours at 150 ℃ to obtain a feed. And (3) loading the feed into a hopper of an injection molding machine, loading a circular blind hole mold with the size of 6mm in diameter, 0.2mm in blind hole depth and 1.5mm in wall thickness into the injection molding machine, and pumping a mold cavity to-0.08 MPa, wherein the mold cavity of the mold is 1mm in thickness and 5.7 inches in size. Setting the temperature of a charging basket of an injection molding machine to be 155 ℃, the injection pressure to be 190MPa for injection molding and the temperature of a mold to be 100 ℃, injecting the molten feed into a mold cavity at a high speed for maintaining the pressure for 1s, and then increasing the mold locking force to 230MPa for shaping and maintaining the pressure for 40s to obtain a regular hexagonal blind hole mobile phone back plate biscuit with the diameter of 6mm, the blind hole depth of 0.2mm and the wall thickness of 1.5 mm.
Stacking the mobile phone backboard biscuit, putting the stack into a degreasing furnace, slowly heating to 170 ℃ at the speed of 0.2 ℃/min, preserving heat for 20h, cooling along with the furnace, stacking the mobile phone backboard biscuit, putting the stack into a sintering furnace, heating to 450 ℃ at the speed of 1 ℃/min, preserving heat for two hours, heating to 650 ℃ at the speed of 1 ℃/min, heating to 1380 ℃ at the speed of 5 ℃/min, preserving heat for 2h, cooling to 950 ℃ at the speed of 5 ℃/min, and cooling along with the furnace to obtain the mobile phone backboard blank.
Weighing 50g of ammonium stearate, adding the ammonium stearate into 3kg of ethanol solution, uniformly mixing, then putting the mobile phone back plate blank into the mobile phone back plate blank, soaking for 3h, putting the mobile phone back plate blank into an oven for drying, then coating liquid epoxy resin into the blind holes, scraping off redundant liquid epoxy resin, curing for 60min at 70 ℃ in the oven, then processing burrs and the balance of the back plate blank by using CNC (computerized numerical control) processing equipment, and then grinding and polishing the blank to obtain the honeycomb blind hole toughened zirconia ceramic mobile phone back plate, wherein the illustration in figure 2 is that.
The samples for testing the bending strength by a three-point bending method and the fracture toughness by a single-side notched beam method require multiple sampling tests to obtain an average value, and the test result shows that the bending strength of the ceramic is 1203MPa, and the fracture toughness is 15.8MPa1/2。
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (10)
1. Cellular blind hole toughened zirconia ceramic cell-phone backplate which characterized in that: more than one periodic regular polygonal blind hole or circular blind hole is formed in the first plane of the zirconia ceramic mobile phone back plate, and organic polymer plastic materials are cured and packaged in the blind holes;
the preparation method of the honeycomb blind hole toughened zirconia ceramic mobile phone back plate comprises the following steps:
a) carrying out high-temperature negative pressure banburying on a surface modifier, inorganic nano zirconia powder, paraffin and an organic high polymer material in a banbury mixer to obtain a feed;
b) injecting the molten feed into a mold with more than one periodic regular polygonal boss or circular boss under the negative pressure of a mold cavity, and performing secondary mold closing, pressurizing and shaping in a semi-molten state to form a back plate biscuit with more than one periodic regular polygonal blind hole or circular blind hole;
c) degreasing, preserving heat and sintering the back plate biscuit to obtain a back plate blank;
d) treating periodic regular polygonal blind holes or circular blind holes of a back plate blank by using a surface modifier;
e) injecting liquid epoxy resin or liquid silica gel into the periodic regular polygonal blind holes or the circular blind holes of the backboard blank treated in the step d), and curing at the temperature of 60-180 ℃ for 5-120 min;
wherein: in the step a), the organic polymer is one of polyethylene, polypropylene and polyphenylene sulfide; the mass percent of the surface modifier is 0.5-0.8%, the mass percent of the inorganic nano zirconia powder is 85.2-92.5%, the mass percent of the paraffin is 4-9%, and the mass percent of the organic polymer is 3-5%; the sintering temperature in the step c) is 1300-1500 ℃, and the heat preservation time is 2-4 h.
2. The cellular blind hole toughened zirconia ceramic mobile phone backboard of claim 1 is characterized in that: the organic polymer plastic material is epoxy resin or silica gel.
3. The cellular blind hole toughened zirconia ceramic mobile phone backboard of claim 2 is characterized in that: the hole depth of the regular polygon blind hole is 0.1 mm-0.9 mm, the side length of the regular polygon blind hole is 0.5 mm-10 mm, and the wall thickness of two adjacent regular polygon blind holes is 0.5 mm-3 mm; the diameter of each circular blind hole is 6mm, the depth of each circular blind hole is 0.2mm, and the wall thickness of each two adjacent circular blind holes is 1.5 mm.
4. The cellular blind hole toughened zirconia ceramic mobile phone backboard of claim 3 is characterized in that: the regular polygon blind hole is one of an equilateral triangle blind hole, a square blind hole, a regular pentagon blind hole and a regular hexagon blind hole.
5. The preparation method of the honeycomb blind hole toughened zirconia ceramic mobile phone back plate of claim 1 is characterized by comprising the following steps:
a) carrying out high-temperature negative pressure banburying on a surface modifier, inorganic nano zirconia powder, paraffin and an organic high polymer material in a banbury mixer to obtain a feed;
b) injecting the molten feed into a mold with more than one periodic regular polygonal boss or circular boss under the negative pressure of a mold cavity, and performing secondary mold closing, pressurizing and shaping in a semi-molten state to form a back plate biscuit with more than one periodic regular polygonal blind hole or circular blind hole;
c) degreasing, preserving heat and sintering the back plate biscuit to obtain a back plate blank;
d) treating periodic regular polygonal blind holes or circular blind holes of a back plate blank by using a surface modifier;
e) and d) injecting liquid epoxy resin or liquid silica gel into the periodic regular polygonal blind holes or the circular blind holes of the backboard blank treated in the step d), and curing at the temperature of 60-180 ℃ for 5-120 min.
6. The preparation method of the honeycomb blind hole toughened zirconia ceramic mobile phone backboard according to claim 5 is characterized in that: the temperature of the mould is 90-120 ℃, the pressure is 150-250 MPa, and the pressure maintaining time is 1 s-2 min during shaping in the step b);
in the step a), the organic polymer is one of polyethylene, polypropylene and polyphenylene sulfide; the mass percent of the surface modifier is 0.5-0.8%, the mass percent of the inorganic nano zirconia powder is 85.2-92.5%, the mass percent of the paraffin is 4-9%, and the mass percent of the organic polymer is 3-5%.
7. The preparation method of the cellular blind hole toughened zirconia ceramic mobile phone backboard according to claim 6 is characterized in that:
the thickness of the back plate biscuit in the step b) is 0.3 mm-2 mm; the hole depth of the regular polygon blind hole obtained by shaping is 0.1-0.9 mm, the side length of the regular polygon blind hole is 0.5-10 mm, the wall thickness of two adjacent regular polygon blind holes is 0.5-3 mm, the diameter of the circular blind hole is 6mm, the depth of the circular blind hole is 0.2mm, and the wall thickness of two adjacent circular blind holes is 1.5mm, wherein the regular polygon blind hole is one of an equilateral triangle blind hole, a square blind hole, a regular pentagon blind hole and a regular hexagon blind hole;
the surface modifier in steps a) and d) is one of stearic acid, ammonium stearate and a silane coupling agent.
8. The preparation method of the cellular blind hole toughened zirconia ceramic mobile phone backboard according to claim 7 is characterized in that: the silane coupling agent is one or the combination of two of gamma-aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane; the inorganic nano zirconia powder is yttrium-stabilized nano zirconia, and the D50 is 30-200 nm.
9. The preparation method of the cellular blind hole toughened zirconia ceramic mobile phone backboard according to claim 8 is characterized in that: in the step a), the banburying temperature is 120-150 ℃, the negative pressure is-0.05 MPa-0.08 MPa, and the banburying time is 1-4 h; the injection molding temperature in the step b) is 130-155 ℃, and the negative pressure is-0.07 MPa to-0.09 MPa.
10. The preparation method of the cellular blind hole toughened zirconia ceramic mobile phone backboard according to claim 9 is characterized in that: the sintering temperature in the step c) is 1300-1500 ℃, and the heat preservation time is 2-4 h.
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