CN107573061A - The manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell and its application - Google Patents
The manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell and its application Download PDFInfo
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Abstract
The invention discloses a kind of manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell and its application.This method sinters base substrate at a temperature of less than ceramic firing makes particle residual adhesion have some strength, density is only 85%~95% biscuit of solid density, densified sintering product again is carved after positive multiform blind hole or blind round hole with carving machine, then filling have cured the organic polymer plastic material such as epoxy resin or silica gel in blind hole.The program is used below firing temperature sintering processing, there is more preferable machinability than injection base substrate, higher processing efficiency and cost advantage are machined with than burning till part, organic polymer plastic material absorbs the impact energy that part is fallen in falling process is collided in blind hole, so as to improve the fracture toughness of ceramic package.The another aspect program can effectively reduce the weight of shell, beneficial to the lightening of electronic product, can be used for preparing the consumer electronics shell such as Watchcase, phone housing, panel housings.
Description
Technical field
The present invention relates to structural member preparation field, and in particular to consumer electronics back board structure part preparation field, more particularly to
The manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell and its application.
Background technology
With the fast development of consumer electronics, the structural member such as shell (backboard) of consumer electronics achieves significantly to enter
Step.Particularly the structure design such as 5G epoch consumer electronics shell when the shield effectiveness that is carried due to it of conventional metals, to antenna
Design brings huge challenge, and plastics its inborn low-intensity shortcomings limit its large scale screen, ultra-thin field should
With in addition as consumers' aesthetic needs to improve, traditional metal shell and plastic casing will be difficult to move consumer.
Because ZrO2 ceramics have high obdurability, good hardness, high-wearing feature, structural ceramics is widely used in
With function ceramics field.Have been reported that PSZ (TZP) by powder metallurgy process, can prepare the hand of corrosion resistant
Table watchcase, table part and Other Instruments part.Therefore in recent years, it is applied to large-sized phone housing also increasing quilt
Researcher is attempted.Such as employed in the patent of Application No. 201510309285.1 in zirconium oxide principal phase add aluminum oxide,
The additives such as titanium oxide prepare phone housing by the way of curtain coating.In another example in the patent of Application No. 201510940002.3
Using the stable zirconia ceramics powder of yttrium and organic matter mixing extrusion shaping mobile phone shell.It is reported that thank to will roc work《Structure
Ceramics》One book introduces the best ZrO of toughness reinforcing performance commercial at present2Ceramic fracture toughness is also only 8~12MPa.m1/2, it is commercial
There are still problem：Zirconia ceramics and metal and plastics ratio, fracture toughness is still bad, and anti-dropping capability is poor, this certainty
Its application is limited, another aspect zirconia ceramics backboard is in order to reach the equal anti-dropping capability of other materials, necessarily using thicker
Ceramics manufacture, notably thickness is more than 1mm for some, and zirconia ceramics density is up to 6.1g/cm3, this necessarily causes zirconium oxide to be made pottery
Porcelain backing is heavy, is not inconsistent with the lightening development path of electronic product.
The content of the invention
In view of this, in view of the existing deficiencies of the prior art, its main purpose is to provide a kind of honeycomb blind hole to the present invention
The manufacture method of toughened zirconium oxide ceramic shell and its application.This method is the interior of honeycomb blind hole toughened zirconium oxide ceramic shell
The multiple regular polygon blind holes of surface engraving or blind round hole, it is organic high that the interior filling of this blind hole have cured epoxy resin or silica gel etc.
Molecule plastic material, organic polymer plastic material absorbs the impact energy fallen of part so as to carry in falling process is collided
High fracture toughness.
To achieve the above object, the present invention is using following technical scheme：A kind of honeycomb blind hole toughened zirconium oxide ceramic
The manufacture method of shell, comprises the following steps：
A) by surface modifier, inorganic nano Zirconium powder, paraffin and high-molecular organic material in banbury high temperature
Negative pressure banburying obtains feeding；
B) step a) is obtained into feeding and shell molds base substrate is injected under mould cavity negative pressure；
C) that shell base substrate that step a) is obtained is accounted for into solid density in high temperature kiln roasting actual density is more than 70% and small
In 85% biscuit of ceramics；
D) in the more than one regular polygon blind hole of the cam plane engraving of biscuit of ceramics first；
E) by biscuit of ceramics treated step d) after 1350 DEG C~1450 DEG C normal pressure heat-insulatings sinter 2h~4h reheating etc.
Static pressure sinters, and 1100 DEG C~1200 DEG C, pressure 50MPa~100MPa of HIP sintering temperature, soaking time is 30min~1h
Obtain backboard blank；
F) using the regular polygon blind hole of surface improver processing backboard blank；
G) injection liquid-state epoxy resin or liquid-state silicon in the regular polygon blind hole of the backboard blank by step f) processing
In 60 DEG C~180 DEG C temperature-curable 5min~120min after glue.
Preferably, sintering temperature is 1200 DEG C~1280 DEG C in step c), and soaking time is 1h~2h.
Preferably, the hole depth of positive shape changeable blind hole is 0.1mm~0.9mm, the side of the regular polygon of regular polygon blind hole
A length of 0.5mm~10mm, the wall thickness of two neighboring regular polygon blind hole is 0.5mm~3mm.
Preferably, regular polygon blind hole is equilateral triangle blind hole, square blind hole, regular pentagon blind hole, regular hexagon
It is a kind of in blind hole and round blind hole.
Preferably, high-molecular organic material is one kind in polyethylene, polypropylene, polyphenylene sulfide in step a), inorganic to receive
Rice Zirconium powder is the stable nano zircite of yttrium, and its D50 is 30nm~200nm.
Preferably, the mass percent of step a) surface modifiers is 0.5%~0.8%, inorganic nano Zirconium powder
Mass percent be 85.2%~92.5%, the mass percent that paraffin is is 4%~9%, organic macromolecule quality hundred
Divide than being 3%~5%.
Preferably, step a) and f) in surface modifier be stearic acid, it is ammonium stearate, a kind of in silane coupler or two
Kind combination.
Preferably, silane coupler is γ-aminopropyl triethoxysilane (KH550), γ-glycidyl ether oxygen propyl
Trimethoxy silane (KH560) and γ-(methacryloxypropyl) propyl trimethoxy silicane (KH570).
Preferably, mixing temperature is 120~150 DEG C in step a), and negative pressure is -0.05MPa~-0.08MPa, mixing time
For 1~4h；Injecting forming temperature is 130~155 DEG C in step b), and negative pressure is -0.07MPa~-0.09MPa.
A kind of phone housing, use the manufacture of the honeycomb blind hole toughened zirconium oxide ceramic shell described in above-mentioned technical proposal
Method is prepared.
Beneficial effects of the present invention：The invention discloses a kind of manufacture method of honeycomb blind hole toughened zirconium oxide ceramic
And its application.This method, which will be molded base substrate and be sintered at a temperature of less than ceramic firing, makes particle residual adhesion have some strength,
After its density is only 70%~85% biscuit of ceramics of solid density, burnt again after carving multiple positive multiform blind holes or blind round hole
Knot is fine and close, and then filling have cured the organic polymer plastic material such as epoxy resin or silica gel in blind hole.The program uses
Sinter and machine less than firing temperature, directly have more preferable machinability than injection base substrate, higher add is machined with than burning till part
Work efficiency rate and cost advantage, organic polymer plastic material absorbs the impact that part is fallen in falling process is collided in blind hole
Energy, so as to improve the fracture toughness of ceramic package.On the other hand because the shell is ceramic and organic matter composite shell, together
The weight of shell can be effectively reduced under equal strength, is advantageous to the lightening development of electronic product.
Brief description of the drawings
Fig. 1 is the manufacture method schematic diagram of honeycomb blind hole toughened zirconium oxide ceramic shell.
Fig. 2 is the schematic diagram of cured epoxy resin gain of heat zirconia ceramics phone housing in cellular regular hexagon blind hole.
Embodiment
The present invention is described in further detail below, wherein used raw material and equipment are commercially available, is not important to
Ask.It is understood that specific embodiment described herein is only used for explaining related invention, rather than the restriction to the invention.
A kind of manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell, is prepared according to the following steps：
A) by surface modifier, inorganic nano Zirconium powder, paraffin and high-molecular organic material in banbury high temperature
Negative pressure banburying obtains feeding.Wherein high-molecular organic material is common polyethylene, polypropylene, makrolon, liquid crystal polymer
Deng organic matter, preferable high-molecular organic material is one kind in polyethylene, polypropylene, polyphenylene sulfide in this example, inorganic to receive
Rice Zirconium powder is the stable nano zircite of yttrium, and its D50 is 30nm~200nm.Surface modifier is stearic acid, stearic acid
One or two kinds of combinations in salt, silane coupler.Wherein, stearate is preferably ammonium stearate, and silane coupler is γ-ammonia
Propyl-triethoxysilicane (KH550), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) and γ-(metering system
Acyl-oxygen) one kind in propyl trimethoxy silicane (KH570).
The mass percent of preferable surface modifier is 0.5%~0.8% in this example, inorganic nano zirconia powder
The mass percent of body is 85.2%~92.5%, and the mass percent that paraffin is is 4%~9%, organic macromolecule quality
Percentage is 3%~5%.
In the present embodiment, different according to above-mentioned preferable component, temperature is 120 DEG C~150 in preferable internal mixing pass
DEG C, negative pressure of vacuum is -0.05MPa~-0.08MPa, and the time is 1h~4h.
B) it will be evacuated in the die cavity of mould after negative pressure state and step a) obtained into banburying feeding injection moulding shell base substrate.
In this example injecting forming temperature be 130 DEG C~155 DEG C, injection before will be evacuated in mould cavity negative pressure -0.07MPa~-
Within 0.09MPa, to reduce injection pressure, the injection base substrate internal flaw such as trace, stomata is reduced, improves blank strength.
C) that shell base substrate that step a) is obtained is accounted for into solid density in high temperature kiln roasting actual density is more than 70% and small
In 85% biscuit of ceramics；Preferably its stacking after degreasing, is transferred to sintering furnace by shell base substrate in debinding furnace in this example
In slowly heating exclude organic polymer framework material after by furnace temperature be warming up to sintering temperature and be incubated a period of time.This insulation is burnt
Junction temperature sinters less than ceramic firing temperature, makes residual adhesion between ceramic particle and particle, turns into the pottery not being densified completely
Porcelain biscuit, because the hardness of biscuit of ceramics is less than the ceramic hardness after burning till, beneficial to machining steps below.According in this example
The difference of material and preparation technology early stage, in order to by blank sintering to more than 70% and less than 85% consistency biscuit of ceramics,
The sintering temperature of this preferable example is 1200 DEG C~1280 DEG C, and soaking time is 1h~2h.
D) in the multiple regular polygon blind holes of the cam plane engraving of biscuit of ceramics first.Preferable first plane is inner surface of outer cover,
Outer surface is complete ceramic surface, is advantageous to attractive in appearance and wear-resisting.Polygonal blind hole can also be carved, is preferably in this example
Regular polygon blind hole, the technique of engraving is carved for CNC or laser engraving.Regular polygon blind hole can be equilateral in this example
It is a kind of or other in triangle blind hole, square blind hole, regular pentagon blind hole, regular hexagon blind hole and round blind hole
Shape, have no special requirement limitation.The hole depth of wherein positive shape changeable blind hole is according to the thickness of shell in 0.1mm~0.9mm
It is preferred that in order to not influence the intensity of shell, the length of side of the regular polygon of preferable regular polygon blind hole is 0.5mm~10mm, phase
The wall thickness of adjacent two regular polygon blind holes is 0.5mm~3mm.
Step d) e) is carved to the biscuit of ceramics densified sintering product after blind hole.Due to biscuit of ceramics have already passed through it is once sintered,
Partial particulate, which has, grows up with adhesion phenomenon, it is necessary to which sintering could be fine and close under higher than 1500 DEG C normal pressures or at higher temperature
Change.Therefore HIP sintering makes its quick densifying again after preferable elder generation is normal pressure-sintered in this example.Preferable ceramics element
HIP sintering obtains backboard blank, HIP sintering to base again after 1350 DEG C~1450 DEG C normal pressure heat-insulatings sinter 2h~4h
1100 DEG C~1200 DEG C, pressure 50MPa~100MPa of temperature, soaking time is 30min~1h.
F) using the regular polygon blind hole of surface improver processing backboard blank, itself and organic polymer plastic material are made
Bond strength is higher, as coming off during.Stearic acid, ammonium stearate, silane coupled is preferably used in this example
The blind hole of one or two kinds of combination modification backboard blanks in agent.
G) injection liquid-state epoxy resin or liquid-state silicon in the regular polygon blind hole of the backboard blank by step f) processing
In 60 DEG C~180 DEG C temperature-curable 5min~120min after glue, liquid resin is set to be cured as organic polymer plastic material, with the back of the body
Plate blank strong bonded.Backboard blank can preferably be added flash and surplus using CNC process equipments in this example
Work is fallen, then by outer surface of outer cover grinding and polishing light processing.
By preparation method technical scheme manufacture phone housing, watchcase, the panel housings of zirconia ceramics shell described above
Deng electronic shell structural member.
It is below the specific embodiment of the present invention：
Embodiment 1
Weigh the 3Y-TZP ceramic powders that γ-(methacryloxypropyl) propyl trimethoxy silicane 14g, D50 is 30nm
1.706kg, No. 58 paraffin 180g and 100g polypropylene, the organic matter weighed is added in 3L banbury and is warming up to 130 DEG C
Make its thawing, then divide 3 times and ceramic powder is added into banburying, treat ceramic powder add after the completion of, by banbury take out negative pressure to-
0.05MPa, feeding is obtained in 135 DEG C of banburying 3h.Feeding is loaded in the hopper of injection machine, by 2.15 inches of Watchcase moulds
Die cavity loads injection machine, and 2.15 inches of Watchcase mould cavities are evacuated into -0.08MPa, set injection machine barrel temperature as 145
DEG C, injection pressure is molded for 180MPa, the feeding of melting is injected pressurize 4s in die cavity at a high speed and obtains Watchcase backboard biscuit.
Watchcase biscuit stacking is put into debinding furnace and is to slowly warm up to 170 DEG C with 0.2 DEG C/min speed, insulation
Furnace cooling after 20h, cell phone back laminin base stacking is put into sintering furnace by 1 DEG C/min, is warming up to 430 DEG C and is incubated two hours,
Then 1 DEG C/min is warming up to 650 DEG C, is cooled to after being then warming up to 1200 DEG C of insulation 2h with 5 DEG C/min speed by 5 DEG C/min
1050 DEG C of furnace coolings obtain the phone housing biscuit of ceramics that consistency is 70.2%.
Watchcase biscuit of ceramics is put into high speed CNC process equipments and accommodated with fixture, with 0.1mm feed velocitys whole
Individual inner surface fluting processing equilateral triangle blind hole, wherein the blind hole length of side 5mm for the equilateral triangle processed, blind hole depth 0.1mm, blind hole
The wall thickness 2mm between blind hole, dried in an oven after it is rinsed with clear water after completion of processing.
The Watchcase biscuit of ceramics of drying is placed after being warming up to 1350 DEG C of insulation 4h in sintering furnace with 5 DEG C/min speed
1050 DEG C of furnace coolings are cooled to by 5 DEG C/min, are then placed within hot isostatic pressure stove, are heated up with 10 DEG C/min speed
To 1100 DEG C, under 100MPa pressure, soaking time is cold with stove to be cooled to 1050 DEG C of furnace coolings by 5 DEG C/min after 30min
But Watchcase blank is obtained.
Weigh γ-aminopropyl triethoxysilane (KH550) 50g and add 2kg deionized waters and 2kg alcohol mixed solutions
In, Watchcase blank is put into after wherein impregnating 2h and is put into oven drying, then coat liquid-state epoxy resin to blind hole
60 DEG C of solidification 120min in an oven are scraped off after unnecessary liquid-state epoxy resin, then backboard blank uses CNC process equipments general
Flash and surplus machine away, and are then handled using ceramic grinding polishing machine and obtain the honeycomb blind hole toughened zirconium oxide ceramic mobile phone
Backboard.
By the more sub-samplings of sample requirement of three-point bending method test bending strength and Single edge notch beam test fracture toughness
Test is averaged, and test result is that the ceramic bending strength is 1213MPa, fracture toughness 15.8MPa.m1/2, and according to thanking
What will roc write《Structural ceramics》One book introduction Y-TZP commercial at present bending strength is usually 800~1200MPa, and fracture is tough
Property is 8~12MPa.m1/2.With the Y-TZP ceramic phases ratio of commercialization, fracture toughness significantly improves, it is particularly suited for phone housing
(backboard).
Embodiment 2
Weigh 3Y-TZP ceramic powder 1.704kg, 180g56 paraffin and 100g that ammonium stearate 16g, D50 are 30nm
Polyethylene, make its thawing by being warming up to 115 DEG C in the organic matter weighed addition 3L banbury, then divide 3 times by ceramic powder
Banburying is added, after the completion for the treatment of that ceramic powder adds, banbury is taken out into negative pressure to -0.05MPa, feeding is obtained in 120 DEG C of banburying 4h.
Feeding is loaded in the hopper of injection machine, be that 5 inches of phone mould die cavitys load injection machine by thickness, by 5 inches of phone moulds
Die cavity is evacuated to -0.09MPa, sets injection machine barrel temperature as 130 DEG C, and injection pressure is molded for 250MPa, makes the feeding of melting
Pressurize 3s obtains cell phone back laminin base in injection die cavity at a high speed.
Cell phone back laminin base stacking is put into debinding furnace is to slowly warm up to 170 DEG C with 0.2 DEG C/min speed, is incubated 20h
Furnace cooling afterwards, cell phone back laminin base stacking is put into sintering furnace by 1 DEG C/min, is warming up to 400 DEG C and is incubated two hours, then
1 DEG C/min is warming up to 650 DEG C, and 1050 DEG C are cooled to by 5 DEG C/min after being then warming up to 1280 DEG C of insulation 1h with 5 DEG C/min speed
Furnace cooling obtains the mobile phone backboard biscuit of ceramics that relative density is 84.7%.
Mobile phone backboard biscuit of ceramics biscuit of ceramics is put into high speed CNC process equipments and accommodated with fixture, with 0.1mm feeds
Speed processes square blind hole in whole inner surface fluting, wherein the square blind hole length of side 0.5mm processed, blind hole are deep
0.1mm, wall thickness 0.5mm between blind hole and blind hole, dried in an oven after it is rinsed with clear water after completion of processing.
The Watchcase biscuit of ceramics of drying is placed after being warming up to 1450 DEG C of insulation 2h in sintering furnace with 5 DEG C/min speed
1050 DEG C of furnace coolings are cooled to by 5 DEG C/min, are then placed within hot isostatic pressure stove, are heated up with 10 DEG C/min speed
To 1200 DEG C, in pressure 50MPa, soaking time is cooled to 1050 DEG C of furnace cooling furnace coolings by 5 DEG C/min after being 1h and obtained
Phone housing blank.
Weigh γ-aminopropyl triethoxysilane 30g and γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560)
20g is added in 2kg deionized waters and 2kg alcohol mixed solutions, is then put into phone housing blank after wherein impregnating 2h and is put into
Oven drying, then liquid-state silicon gel is coated to scraping off 180 DEG C of solidifications in an oven after unnecessary liquid-state silicon gel resin in blind hole
5min, then backboard blank flash and surplus are machined away using CNC process equipments, then using ceramic grinding polishing machine handle be
Obtain the honeycomb blind hole toughened zirconium oxide ceramic mobile phone backboard.
By the more sub-samplings of sample requirement of three-point bending method test bending strength and Single edge notch beam test fracture toughness
Test is averaged, and test result is that the ceramic bending strength is 1143MPa, fracture toughness 14.0MPa.m1/2。
Embodiment 3
Stearic acid 10g, D50 are weighed as 200nm 3Y-TZP ceramic powder 1.85kg, 80g58 paraffin and 60g polyphenyl
Thioether, make its thawing by being warming up to 120 DEG C in the organic matter weighed addition 3L banbury, then divide 3 times and add ceramic powder
Enter banburying, after the completion for the treatment of that ceramic powder adds, banbury is taken out into negative pressure to -0.08MPa, feeding is obtained in 150 DEG C of banburying 1h.Will
Feeding loads in the hopper of injection machine, is that 8 inch flat panel die cavitys load injection machine by thickness, 8 inch flat panel mould cavities are taken out
To -0.07MPa, injection machine barrel temperature is set as 155 DEG C, and injection pressure is molded for 200MPa, the feeding of melting is noted at a high speed
Enter pressurize 5s in die cavity and obtain panel housings biscuit.
Panel housings biscuit stacking is put into debinding furnace is to slowly warm up to 170 DEG C with 0.2 DEG C/min speed, is incubated 20h
Furnace cooling afterwards, flat board backboard biscuit stacking is put into sintering furnace by 1 DEG C/min, is warming up to 450 DEG C and is incubated two hours, then
1 DEG C/min is warming up to 650 DEG C, and 1050 DEG C are cooled to by 5 DEG C/min after being then warming up to 1250 DEG C of insulation 2h with 5 DEG C/min speed
Furnace cooling obtains the panel housings biscuit of ceramics that relative density is 80.5%.
Panel housings biscuit of ceramics is put into high speed CNC process equipments and accommodated with fixture, with 0.3mm depths of cut whole
Individual inner surface opens milling regular pentagon blind hole, wherein the blind hole length of side 10mm of the regular pentagon of milling, blind hole depth 0.9mm, blind hole with it is blind
Wall thickness 3mm between hole, dried in an oven after it is rinsed with clear water after completion of processing.
The panel housings biscuit of ceramics of drying is placed after being warming up to 1400 DEG C of insulation 3h in sintering furnace with 5 DEG C/min speed
1050 DEG C of furnace coolings are cooled to by 5 DEG C/min, are then placed within hot isostatic pressure stove, are heated up with 10 DEG C/min speed
To 1150 DEG C, in pressure 100MPa, soaking time is cooled to 1050 DEG C of furnace cooling furnace coolings by 5 DEG C/min after being 1h and obtained
Panel housings blank.
Weigh γ-(methacryloxypropyl) propyl trimethoxy silicane 50g and add 2kg deionized waters and the mixing of 2kg ethanol
In solution, then panel housings blank is put into after wherein impregnating 2h and is put into oven drying, then coat liquid-state silicon gel to blind
180 DEG C of solidification 10min in an oven are scraped off after unnecessary liquid-state silicon gel in hole, then panel housings blank is set using CNC processing
It is standby to machine away flash and surplus, then handled using ceramic grinding polishing machine and obtain the honeycomb blind hole toughened zirconium oxide ceramic
Panel housings.
By the more sub-samplings of sample requirement of three-point bending method test bending strength and Single edge notch beam test fracture toughness
Test is averaged, and test result is that the ceramic bending strength is 1077MPa, fracture toughness 14.5MPa.m1/2。
Embodiment 4
Weigh γ-aminopropyl triethoxysilane 12g, D50 be 50nm 8Ce-TZP ceramic powders 1.708kg, No. 58
Paraffin 180g and 100g polypropylene, make its thawing by being warming up to 130 DEG C in the organic matter weighed addition 3L banbury, then
Divide 3 times and ceramic powder is added into banburying, after the completion for the treatment of that ceramic powder adds, banbury is taken out into negative pressure to -0.07MPa, at 140 DEG C
Banburying 3h obtains feeding.Feeding is loaded in the hopper of injection machine, 6 inches of phone mould die cavitys that thickness is 0.6mm are loaded
Injection machine, 6 inches of phone mould die cavitys are taken out into negative pressure to -0.08MPa, set injection machine barrel temperature as 150 DEG C, injection pressure
It is molded for 190MPa, the feeding of melting is injected pressurize 4s in die cavity at a high speed and obtain 6 cun of phone housing biscuits.
Phone housing biscuit stacking is put into debinding furnace is to slowly warm up to 170 DEG C with 0.2 DEG C/min speed, is incubated 20h
Furnace cooling afterwards, phone housing biscuit stacking is put into sintering furnace by 1 DEG C/min, is warming up to 420 DEG C and is incubated two hours, then
1 DEG C/min is warming up to 650 DEG C, and 1050 DEG C are cooled to by 5 DEG C/min after being then warming up to 1270 DEG C of insulation 1h with 5 DEG C/min speed
Furnace cooling obtains the phone housing biscuit of ceramics that relative density is 83.2%.
Phone housing biscuit of ceramics is put into high speed CNC process equipments and accommodated with fixture, with 0.3mm depths of cut whole
Blind hole length of side 3mm, the blind hole depth 0.3mm of individual inner surface milling regular hexagon blind hole, the wherein regular hexagon of milling, blind hole and blind hole it
Between wall thickness 2mm, dried in an oven after it is rinsed with clear water after completion of processing.
The panel housings biscuit of ceramics of drying is placed in sintering furnace 1400 DEG C of insulation 2.5h are warming up to 5 DEG C/min speed
1050 DEG C of furnace coolings are cooled to by 5 DEG C/min afterwards, are then placed within hot isostatic pressure stove, with 10 DEG C/min speed liter
Temperature is to 1150 DEG C, and in pressure 50MPa, soaking time is cooled to 1050 DEG C of furnace cooling furnace coolings by 5 DEG C/min after being 1h and obtained
To mobile phone outer sleeve blank.
Weigh and be well mixed in stearic acid 50g addition 3kg ethanol solutions, then mobile phone backboard blank is put into and wherein impregnated
Oven drying is put into after 3h, then coats liquid-state epoxy resin to scraping off in blind hole after unnecessary liquid-state epoxy resin in baking oven
In 80 DEG C solidification 40min, then backboard blank flash and surplus are machined away using CNC process equipments, then using ceramic grinding
Polishing machine processing obtains the honeycomb blind hole toughened zirconium oxide ceramic phone housing, as shown in Figure 2.
By the more sub-samplings of sample requirement of three-point bending method test bending strength and Single edge notch beam test fracture toughness
Test is averaged, and test result is that the ceramic bending strength is 1095MPa, fracture toughness 14.9MPa.m1/2。
Embodiment 5
Weigh γ-glycidyl ether oxygen propyl trimethoxy silicane 8g, γ-(methacryloxypropyl) propyl trimethoxy silicon
Alkane 6g, D50 are 30nm 3Y-TZP ceramic powders 1.766kg, No. 56 paraffin 140g and 80g polyphenylene sulfide, are had what is weighed
Being warming up to 145 DEG C in machine thing addition 3L banbury makes its thawing, then divides 3 times ceramic powder adding banburying, treat ceramic powder
After the completion of body adds, banbury is taken out into negative pressure to -0.06MPa, feeding is obtained in 150 DEG C of banburying 2h.Feeding is loaded into injection machine
Hopper in, 5.7 inches of phone mould die cavitys are loaded into injection machines, 5.7 inches of phone mould die cavitys are evacuated to -0.08MPa, if
Injection machine barrel temperature is determined for 155 DEG C, and injection pressure is molded for 190MPa, the feeding of melting is injected pressurize 4s in die cavity at a high speed
Obtain phone housing biscuit.
Phone housing biscuit stacking is put into debinding furnace is to slowly warm up to 170 DEG C with 0.2 DEG C/min speed, is incubated 20h
Furnace cooling afterwards, cell phone back laminin base stacking is put into sintering furnace by 1 DEG C/min, is warming up to 450 DEG C and is incubated two hours, then
1 DEG C/min is warming up to 650 DEG C, and 1050 DEG C are cooled to by 5 DEG C/min after being then warming up to 1230 DEG C of insulation 1h with 5 DEG C/min speed
Furnace cooling obtains the mobile phone backboard blank that relative density is 76.6%.
Phone housing biscuit of ceramics is put into high speed CNC process equipments and accommodated with fixture, with 0.2mm depths of cut whole
Individual inner surface processes blind round hole, wherein a diameter of 7mm of the blind round hole processed, blind hole depth 0.2mm, the partition of blind hole and blind hole
Thick 1.5mm, dried in an oven after it is rinsed with clear water after completion of processing.
The phone housing biscuit of ceramics of drying is placed after being warming up to 1380 DEG C of insulation 3h in sintering furnace with 5 DEG C/min speed
1050 DEG C of furnace coolings are cooled to by 5 DEG C/min, are then placed within hot isostatic pressure stove, are heated up with 10 DEG C/min speed
To 1150 DEG C, in pressure 100MPa, soaking time by 5 DEG C/min is cooled to 1050 DEG C of furnace cooling furnace coolings after being 30min
Obtain phone housing blank.
Weigh and be well mixed in ammonium stearate 50g addition 3kg ethanol solutions, then mobile phone backboard blank is put into and wherein soaked
Oven drying is put into after stain 3h, then liquid-state epoxy resin is coated to after scraping off unnecessary liquid-state epoxy resin in blind hole and dried
70 DEG C solidify 60min in case, and then backboard blank is machined away flash and surplus using CNC milling cutters, then using ceramic grinding and polishing
Light processing obtains the honeycomb blind hole toughened zirconium oxide ceramic mobile phone backboard.
By the more sub-samplings of sample requirement of three-point bending method test bending strength and Single edge notch beam test fracture toughness
Test is averaged, and test result is that the ceramic bending strength is 1219MPa, fracture toughness 15.6MPa.m1/2。
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology that the particular combination of above-mentioned technical characteristic forms
Scheme, while should also cover in the case where not departing from the inventive concept, carried out by above-mentioned technical characteristic or its equivalent feature
The other technical schemes for being combined and being formed.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical scheme that the technical characteristic of energy is replaced mutually and formed.
Claims (10)
1. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell, it is characterised in that comprise the following steps：
A) by surface modifier, inorganic nano Zirconium powder, paraffin and high-molecular organic material in banbury high temperature negative pressure
Banburying obtains feeding；
B) step a) is obtained into feeding and shell molds base substrate is injected under mould cavity negative pressure；
C) the shell base substrate that step a) is obtained is accounted for into solid density more than 70% in high temperature kiln roasting actual density and be less than
85% biscuit of ceramics；
D) in the more than one regular polygon blind hole of the cam plane engraving of biscuit of ceramics first；
E) by biscuit of ceramics treated step d) after 1350 DEG C~1450 DEG C normal pressure heat-insulatings sinter 2h~4h high temperature insostatic pressing (HIP) again
Sintering, 1100 DEG C~1200 DEG C, pressure 50MPa~100MPa of HIP sintering temperature, soaking time are that 30min~1h is obtained
Backboard blank；
F) using the regular polygon blind hole of surface improver processing backboard blank；
G) after injecting liquid-state epoxy resin or liquid-state silicon gel in the regular polygon blind hole of the backboard blank handled by step f)
In 60 DEG C~180 DEG C temperature-curable 5min~120min.
2. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 1, it is characterised in that：Step
It is rapid c) in sintering temperature be 1200 DEG C~1280 DEG C, soaking time is 1h~2h.
3. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 2, it is characterised in that：Just
The hole depth of shape changeable blind hole is 0.1mm~0.9mm, and the length of side of the regular polygon of regular polygon blind hole is 0.5mm~10mm, phase
The wall thickness of adjacent two regular polygon blind holes is 0.5mm~3mm.
4. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 3, it is characterised in that：Just
Polygonal blind hole is one in equilateral triangle blind hole, square blind hole, regular pentagon blind hole, regular hexagon blind hole and round blind hole
Kind.
5. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 4, it is characterised in that：Step
It is rapid a) in high-molecular organic material be polyethylene, polypropylene, one kind in polyphenylene sulfide, inorganic nano Zirconium powder is that yttrium is steady
Determine nano zircite, its D50 is 30nm~200nm.
6. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 5, it is characterised in that：Step
It is rapid a) in the mass percent of surface modifier be 0.5%~0.8%, the mass percent of inorganic nano Zirconium powder is
85.2%~92.5%, the mass percent that paraffin is is 4%~9%, and organic macromolecule mass percent is 3%~5%.
7. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 6, it is characterised in that：Step
It is rapid a) and f) in surface modifier be stearic acid, one or two kinds of combinations of ammonium stearate, silane coupler.
8. the manufacture method of honeycomb blind hole toughened zirconium oxide ceramic shell according to claim 7, it is characterised in that：Silicon
Alkane coupling agent is γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane and γ-(methyl-prop
Alkene acyl-oxygen) one kind in propyl trimethoxy silicane.
9. the preparation method of honeycomb blind hole toughened zirconium oxide ceramic mobile phone backboard according to claim 8, its feature exist
In：Mixing temperature is 120 DEG C~150 DEG C in step a), and negative pressure is -0.05MPa~-0.08MPa, and mixing time is 1~4h；Step
It is rapid b) in injecting forming temperature be 130 DEG C~155 DEG C, negative pressure is -0.07MPa~-0.09MPa.
A kind of 10. phone housing, it is characterised in that manufacturer's legal system of any claim described in usage right requirement 1~9
It is standby to obtain.
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