CN110105071A - A kind of preparation method and its mobile phone backboard of silicified wood surface structure part - Google Patents
A kind of preparation method and its mobile phone backboard of silicified wood surface structure part Download PDFInfo
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of preparation method of silicified wood ceramics surface structure and its mobile phone backboards, it is to hydrolyze to obtain silica offer silicon source by wood matrix absorption ethyl orthosilicate and (or) butyl silicate, porous lumber fibre structure is carbonized in a nitrogen atmosphere provides carbon source, silicon source, the silicon powder or silicon monoxide of carbon source and sintering process grow to obtain silicon carbide in nitrogen atmosphere along the own fibre structure shape of timber, the compound silicified wood ceramics surface structure part of the components such as silicon nitride and silica, the surface structure part is not merely with the distinctive microstructure of lumber fibre, excellent in mechanical performance, and surface has wood fibre structural style, solve zirconia ceramics shell, the single problem of structure color, meet the consumption demand of multiplicity.
Description
Technical field
The present invention relates to structural member preparation fields, and in particular to consumer electronics back board structure part preparation field, in particular to
A kind of preparation method and its mobile phone backboard of silicified wood surface structure part.
Background technique
With the fast development of the consumer electronics such as mobile phone, the structural members such as shell (backboard) of consumer electronics achieve considerable
Progress, but also encounter new problem.Especially 5G epoch in the future material that offsets power-consuming subshell (backboard) proposes harsher
Requirement.Conventional metals bring huge challenge due to its shield effectiveness, to Antenna Design, would be unavailable for 5G shell (back
Plate) manufacture, and plastics its low-intensity, it is not wear-resisting limit it in the application in large scale screen, ultra-thin field, in addition with
Aesthetic raising is consumed, the shell (backboard) of tradition single metal shell and plastic material will also be difficult to move consumer.
Due to ZrO2Ceramics and Al2O3Ceramics have high obdurability, good bending strength, are widely used in structure
Ceramics and function ceramics field.Also have been reported that partially stabilized zirconia (TZP) can prepare hand by powder metallurgy process
The table part and Other Instruments part of table watchcase, corrosion resistant.Therefore in recent years, it is applied to phone housing and is also more and more ground
The person of studying carefully is attempted.Such as application No. is use to add aluminium oxide, oxygen in zirconium oxide main phase in 201510309285.1 patent
Change the additives such as titanium and prepares phone housing by the way of curtain coating.But simple ZrO2 ceramic density is big, product is heavy, raw material at
This height leads to the high expensive of the structural members such as phone housing.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of silicified wood ceramics
The preparation method of surface structure, comprising the following steps:
A) timber adsorbs in ethyl orthosilicate and (or) butyl silicate solution；
B) will through in the processed timber of step a) ethyl orthosilicate and (or) butyl silicate hydrolyze；
C) it is carbonized under the conditions of oxygen barrier through the processed timber of step b) and obtains biscuit；
D) biscuit and silicon powder and (or) silicon monoxide are sintered under the conditions of nitrogen atmosphere and obtain the ceramics surface structure part.
It preferably, further include the non-fibres such as extract, lignin in the removal timber removed in timber before step a)
The compound for tieing up structure, forms the step 1) of the timber of porous structure.
Preferably, step 1) process is that timber is immersed in 20 DEG C~90 DEG C of hydrochloric acid and the mixed liquor of hydrogen peroxide
In.
Preferably, step 1) soaking technology method is that pressurization is impregnated, and immersion pressure is 0MPa~2.5MPa.
Preferably, step a) timber absorbing process is that pressurization is immersed in ethyl orthosilicate and (or) butyl silicate solution
In, immersion pressure is 0MPa~1MPa.
Preferably, step b) uses steam hydrolysis, and hydrolysis temperature is 60 DEG C~105 DEG C, and hydrolysis time is 1h~48h.
Preferably, be carbonized oxygen barrier technique of step c) is that nitrogen atmosphere is oxygen barrier, be carburizing temperature is 800 DEG C~1100 DEG C, carbon
The change time is 1h~40h.
Preferably, the molar ratio in step d) being silicon powder and silicon monoxide is 0.5~3, sintering temperature is 1300 DEG C~
1550 DEG C, 1~6h of sintering time.
Preferably, the molar ratio in step d) being silicon powder and silicon monoxide is 0.7~1.5, sintering temperature is 1350 DEG C~
1450 DEG C, 2~4h of sintering time.
A kind of mobile phone backboard is after timber is processed into hemizygous closed structure, is prepared into using above-mentioned preparation method
It arrives.
Beneficial effects of the present invention: the invention discloses a kind of preparation methods of silicified wood ceramics surface structure, are logical
It crosses timber absorption ethyl orthosilicate and (or) butyl silicate hydrolyzes to obtain silica offer silicon source, porous lumber fibre structure
In a nitrogen atmosphere carbonization provide carbon source, silicon source, the silicon powder of carbon source and sintering process or silicon monoxide nitrogen atmosphere along
The own fibre structure shape of timber grows to obtain the compound silicified wood ceramics appearance knot of silicon carbide, silicon nitride and silica
Component, the surface structure part do not have wood merely with the distinctive microstructure of lumber fibre, excellent in mechanical performance, and surface
Matter fibre structure pattern, solves zirconia ceramics shell, and the single problem of structure color meets the consumption demand of multiplicity.
Detailed description of the invention
Fig. 1 is phone housing (Watchcase) preparation technology flow chart of embodiment.
Specific embodiment
Present invention is further described in detail below, wherein used raw material and equipment be it is commercially available, be not important to
It asks.It is understood that specific embodiment described herein is only used for explaining related invention, rather than the restriction to the invention.
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of silicified wood ceramics
The preparation method of surface structure, comprising the following steps:
A) timber adsorbs in ethyl orthosilicate and (or) butyl silicate solution.Ethyl orthosilicate in the present embodiment
Both and (or) butyl silicate solution can be pure teos solution, pure butyl silicate solution, be also possible to
The ethyl orthosilicate and (or) butyl silicate solution of mixing or aqueous and other solution, such as can be ethyl orthosilicate
And (or) butyl silicate solution water and mixed alkoxide solution.
If ethyl orthosilicate and (or) butyl silicate solution water and mixed alkoxide solution, preparation method in the present embodiment
It is as follows: to be calculated with volume ratio, take 4~8 parts of ethyl orthosilicate and (or) butyl silicate, 1~3 part of water, be put into solvent
Stirring, it is 1~6 that acid for adjusting pH value, which is added, is added 1~3 part of ethyl alcohol, is warming up to 70~80 DEG C, reacts 0.5h~1.5h, and ammonia is added
Water adjusts pH value to 7~12, continues 0.5~1.5h of stirring and completes solution preparation.
In order to promote ethyl orthosilicate and (or) butyl silicate solution water before step a) preferred in this embodiment
Alcoholic solution adsorbance further includes the non-fiber such as extract, lignin in the removal timber removed in timber before step a)
The compound of structure forms the step 1) of the timber of porous structure, and process can be in the prior art.The present embodiment is mentioned
Extract refer in timber to include that resin, natural gum, essential oil, pigment, alkaloid, fat, wax, sugar, starch and silicide etc. are multiple
Close object.
In the present embodiment further process be timber is immersed in 20 DEG C~90 DEG C hydrochloric acid and hydrogen peroxide it is mixed
It closes and impregnates 2h~100h in liquid, so that the non-woods structural compounds removal such as ketone and lipid in timber, preferred to soak
Steeping temperature is 50~75 DEG C, and the ratio of hydrochloric acid and hydrogen peroxide is hydrochloric acid and hydrogen peroxide mixing quality concentration 20 between 0.5~2.5
Between~60%.Further preferred soaking technology method is that pressurization is impregnated, and immersion pressure is 0~2.5MPa, in the work of pressure
Under, hydrochloric acid and hydrogen peroxide are rapidly entered in timber gap, promotes the removal non-wood-fibers knot such as ketone and lipid
The compound of structure.
In this example, timber absorption ethyl orthosilicate and (or) butyl silicate solution process are closed to place timber
It is pressurizeed in soaking solution in container, immersion moulding pressure is 0~1MPa, passes through the solution for impregnating and can making to promote timber that pressurizes
Adsorbance.Timber can be further placed on in closed container first negative pressure and pump air etc. in timber, then pressurizeed
Dipping further promotes absorbent solution ability.
Preferred ethyl orthosilicate and (or) butyl silicate solution are pure ethyl orthosilicate and positive silicon in this example
The mixed solution of acid butyl ester solution.
B) by through in the processed timber of step a) ethyl orthosilicate and (or) butyl silicate hydrolyze to obtain silica
Silicon source is provided for subsequent reactions.Hydrolysis is participated in using vapor in this example, vapor can be used normal heating, subtract
Realization that pressure heats or the method for other such as compressed airs makes water fogging.Hydrolysis temperature in this example is 60~105 DEG C, into
The hydrolysis temperature of one step is 70~85 DEG C, and hydrolysis time is 1h~48h, and further hydrolysis time is 4h~12h.
C) it is carbonized under the conditions of oxygen barrier through the processed timber of step b) and obtains biscuit.Timber after hydrolyzed is placed on burning
The effect for passing through starvation atmosphere in freezing of a furnace, wood fibre is carbonized under high temperature action, provides carbon source for subsequent reactions.Every
Vacuum condition in the prior art or inert atmosphere conditions can be used in exhausted oxygen atmosphere, select nitrogen in the present embodiment
Atmospheric condition, by nitrogen purging effect in sintering furnace, by carbonisation, other elements are purged away other than carbon, are added
Fast carbonisation promotes carbonation rate.It is in this example further carburizing temperature is 800 DEG C~1100 DEG C, carbonization time 1h
~40h, further carburizing temperature be 800~850 DEG C, 20~35h of carbonization time, select lower carburizing temperature and it is long when
Between be carbonized so that timber is unlikely to the defects of flash carbonization cracking, damaged occur, can further be promoted to obtain surface structure part
Performance.Heating rate is 3~5 during from room temperature to carburizing temperature in further carbonisation in the present embodiment
℃/min。
D) biscuit and silicon powder and (or) silicon monoxide are sintered under the conditions of oxygen barrier and obtain the ceramics surface structure part.At this
Carbonization biscuit is obtained in example to be put into sintering furnace, nitrogen atmosphere effect under so that carbon, silica, silicon, silicon monoxide with
Nitrogen reaction, so that silicon carbide, silicon nitride obtain compound surface structure along the wood grain structure growth of timber biscuit
Part.Sintering temperature sintering temperature is 1300 DEG C~1550 DEG C, 1~6h of sintering time in the present embodiment, further sintering temperature
Spending sintering temperature is 1350 DEG C~1450 DEG C, and 2~4h of sintering time enables reactant more fully to grow, and is unlikely to
Crystal grain grow up it is too fast, formed abnormal growth, influence final performance.Further rubbing for silicon powder and silicon monoxide in this embodiment
You, so that react generation hydrocarbon with oxygen by carbon containing aerobic in element, remove surface structure part and are more than than being 0.5~3
Carbon, the molar ratio of further silicon powder and silicon monoxide is 0.7~1.5, effectively inhibits sintering process in this range
Middle silicon powder melts, and reduces the adhesion with surface structure, promotes the surface topography of surface structure.
It is the embodiment of the present invention below:
Embodiment 1
Paulownia wood timber is cut into 5.5 cun of phone housing size shapes using CNC, its normal pressure is immersed in ethyl orthosilicate
With butyl silicate solution water and mixed alkoxide solution dipping 48h (mixed solution is prepared by method in specific embodiment).Then
It is dried after timber backboard after dipping to be put into the gaseous mixture hydrolysis 48h for being passed through water and air in 60 DEG C of baking oven.Weighing 5.5 cun of hands of ratio
Machine shell weight gain 5.2%.Then the timber backboard after drying is put into atmosphere sintering furnace to be passed through in nitrogen atmosphere to be added with 3 DEG C/min
Cool down after entering to 800 DEG C of heat preservation 40h with furnace.Timber backboard embedment silicon powder/silicon monoxide=0.5 after carbonization is with 5 DEG C/min
Heating rate is warming up to furnace cooling after 1550 DEG C of heat preservation 1h.Using machine-tooled method finished surface, then by its surface polishing,
The phone housing of the silication timber structure is obtained.
In order to test the silicified wood mobile phone backboard mechanical property, three-point bending method and unilateral notch are prepared by same technique
Multiple samples of beam method test carry out Mechanics Performance Testing, the results showed that the bending strength of the ceramics is 870MPa, fracture toughness
For 6.5MPa.m1/2.It is usually according to the bending strength for thanking to the current commercial Y-TZP of " structural ceramics " book introduction that will roc writes
800~1200MPa, fracture toughness are 8~12MPa.m1/2.Compared with commercial Y-TZP, main mechanical properties connects with it
Closely, there is good wood grain structure, it is apparent beautiful, it is suitble to the requirement of mobile phone backboard surface structure part.
Embodiment 2
Paulownia wood timber is cut into 1.5 cun of Watchcase size shapes using CNC, is immersed in ethyl alcohol, water and hydrogen-oxygen
Change 20 DEG C of immersion 36h drying removal extracts of normal pressure and lignin, rear loss of weight 11.2% of weighing in the mixed solution of sodium.
Then it is impregnated into 36h in teos solution in 1MPa pressure impregnation.Then timber backboard after dipping is put
It is dried after entering to be passed through the gaseous mixture hydrolysis 1h of water and air in 105 DEG C of baking oven, weighing after removal extract and lignin than increasing weight
7.8%.Then the timber backboard after drying, which is put into atmosphere sintering furnace to be passed through in nitrogen atmosphere, to be added with 3 DEG C/min to 1100 DEG C
Cool down after heat preservation 1h with furnace.Timber backboard embedment silicon powder/silicon monoxide=3 after carbonization are with the heating of 5 DEG C/min heating rate
Furnace cooling after to 1300 DEG C of heat preservation 6h.Using machine-tooled method finished surface, then by its surface polishing, silicified wood has been obtained
Watchcase.
In order to test the silicified wood Watchcase mechanical property, three-point bending method and unilateral notch are prepared by same technique
Multiple samples of beam method test carry out Mechanics Performance Testing, the results showed that the bending strength of the ceramics is 926MPa, fracture toughness
For 7.5MPa.m1/2.It is estimated with good wood grain structure, apparent beautiful, suitable Watchcase surface structure part requirement.
Embodiment 3
Paulownia wood timber is cut into 1.5 cun of Watchcase size shapes using CNC, is immersed in hydrochloric acid and hydrogen peroxide
20 DEG C of immersion 36h drying removal extracts of normal pressure and lignin in the mixed liquor mixed solution of (hydrochloric acid: hydrogen peroxide=1:1), after
Weighing loss of weight 20.8%.
Then it is impregnated into 36h in teos solution in 1MPa pressure impregnation.Then timber backboard after dipping is put
It is dried after entering to be passed through the gaseous mixture hydrolysis 1h of water and air in 105 DEG C of baking oven, weighing after removal extract and lignin than increasing weight
11.7%.Then the timber backboard after drying, which is put into atmosphere sintering furnace to be passed through in nitrogen atmosphere, to be added with 3 DEG C/min to 900 DEG C
Cool down after heat preservation 3h with furnace.Timber backboard embedment silicon powder/silicon monoxide=0.7 after carbonization is with 5 DEG C/min heating rate liter
Furnace cooling after temperature to 1350 DEG C of heat preservation 4h.Using machine-tooled method finished surface, then by its surface polishing, silication has been obtained
The wooden Watchcase.
In order to test the silicified wood Watchcase mechanical property, three-point bending method and unilateral notch are prepared by same technique
Multiple samples of beam method test carry out Mechanics Performance Testing, the results showed that the bending strength of the ceramics is 1049MPa, fracture toughness
For 7.9MPa.m1/2.It is estimated with good wood grain structure, apparent beautiful, suitable Watchcase surface structure part requirement.
Embodiment 4
Paulownia wood timber is cut into 5 cun of phone housing size shapes using CNC, is immersed in hydrochloric acid and hydrogen peroxide (salt
Acid: hydrogen peroxide=2:1) mixed liquor under 1.5MPa pressure 90 DEG C of immersions 12h drying removal extracts and lignin, rear title
Weight loss of weight 22.4%.
Then it is impregnated into 36h in butyl silicate solution in 1MPa pressure impregnation.Then timber backboard after dipping is put
It is dried after entering to be passed through the gaseous mixture hydrolysis 10h of water and air in 80 DEG C of baking oven, weighing after removal extract and lignin than increasing weight
14.3%.Then the timber backboard after drying, which is put into atmosphere sintering furnace to be passed through in nitrogen atmosphere, to be added with 5 DEG C/min to 1000
DEG C heat preservation 3h after cool down with furnace.Timber backboard embedment silicon powder/silicon monoxide=1.5 after carbonization are with 5 DEG C/min heating rate
It is warming up to furnace cooling after 1450 DEG C of heat preservation 3h.Using machine-tooled method finished surface, then by its surface polishing, it is somebody's turn to do
The phone housing of silication timber structure.
In order to test 5 cun of phone housing mechanical properties of the silicified wood, three-point bending method and unilateral is prepared by same technique
Multiple samples of coped beam method test carry out Mechanics Performance Testing, the results showed that the bending strength of the ceramics is 1178MPa, fracture
Toughness is 9.5MPa.m1/2.It is estimated with good wood grain structure, apparent beautiful, suitable Watchcase surface structure part requirement.
Embodiment 5
Ash timber is cut into 6.5 cun of phone housing size shapes using CNC, is immersed in hydrochloric acid and hydrogen peroxide
70 DEG C of immersion 12h drying remove extracts and lignin under 2.5MPa pressure in the mixed liquor of (hydrochloric acid: hydrogen peroxide=2:1),
Weighing loss of weight 18.1% afterwards.
Then by it in 1MPa pressure impregnation in ethyl orthosilicate and butyl silicate solution (ethyl orthosilicate: positive silicic acid
Butyl acetate solution=3:1) dipping 20h.Then timber backboard after dipping is put into the gaseous mixture that water and air is passed through in 80 DEG C of baking oven
It is dried after hydrolysis 15h, weighing is than increasing weight 13.8% after removal extract and lignin.Then the timber backboard after drying is put into gas
It is passed through in atmosphere sintering furnace in nitrogen atmosphere after being added with 5 DEG C/min to 1000 DEG C of heat preservation 3h and cools down with furnace.Timber back after carbonization
Plate is embedded to silicon powder/silicon monoxide=1.5 and is warming up to furnace cooling after 1400 DEG C of heat preservation 4h with 5 DEG C/min heating rate.It uses
Machine-tooled method finished surface has obtained the phone housing of the silication timber structure then by its surface polishing.
In order to test 5 cun of phone housing mechanical properties of the silicified wood, three-point bending method and unilateral is prepared by same technique
Multiple samples of coped beam method test carry out Mechanics Performance Testing, the results showed that the bending strength of the ceramics is 1252MPa, fracture
Toughness is 10.6MPa.m1/2.It is estimated with good wood grain structure, apparent beautiful, suitable Watchcase surface structure part is wanted
It asks.
Above embodiments, which compare, can see, and Examples 1 to 5 is able to achieve the application, and the best performance of embodiment 5 is real
Example 1 is applied compared with 2, increases the process of removal extract and lignin, ethyl orthosilicate and butyl silicate can be obviously improved
Solution adsorbance implements 2 compared with 3, the removal effect of hydrochloric acid and hydrogen peroxide mixed soaking solution is wanted to promote the effect of hydrolysis
Go eradicating efficacy good than alcohol and sodium hydrate aqueous solution.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (10)
1. a kind of preparation method of silicified wood ceramics surface structure part, which comprises the following steps:
A) timber adsorbs in ethyl orthosilicate and (or) butyl silicate solution；
B) will through in the processed timber of step a) ethyl orthosilicate and (or) butyl silicate hydrolyze；
C) it is carbonized under the conditions of oxygen barrier through the processed timber of step b) and obtains biscuit；
D) biscuit and silicon powder and (or) silicon monoxide are sintered under the conditions of nitrogen atmosphere and obtain the ceramics surface structure part.
2. the preparation method of silicified wood ceramics surface structure part according to claim 1, which is characterized in that step a) it
Before, further include the compound of the non-fibrous structures such as extract, lignin in removal timber, forms the step of the timber of porous structure
It is rapid 1).
3. the preparation method of silicified wood ceramics surface structure part according to claim 2, which is characterized in that step 1) technique
Method be by timber be immersed in 20 DEG C~90 DEG C of hydrochloric acid and the mixed liquor of hydrogen peroxide in.
4. the preparation method of silicified wood ceramics surface structure according to claim 3, which is characterized in that step 1) impregnates work
Process is that pressurization is impregnated, and immersion pressure is 0MPa~2.5MPa.
5. the preparation method of silicified wood ceramics surface structure part according to claim 4, which is characterized in that step a) timber
Absorbing process is that pressurization is immersed in ethyl orthosilicate and (or) butyl silicate solution, and immersion pressure is 0MPa~1MPa.
6. the preparation method of silicified wood ceramics surface structure part according to claim 5, which is characterized in that step b) is used
Steam hydrolysis, hydrolysis temperature are 60 DEG C~105 DEG C, and hydrolysis time is 1h~48h.
7. the preparation method of silicified wood ceramics surface structure part according to claim 6, which is characterized in that step c) carbonization
Oxygen barrier technique is that nitrogen atmosphere is oxygen barrier, be carburizing temperature is 800 DEG C~1100 DEG C, and carbonization time is 1h~40h.
8. the preparation method of silicified wood ceramics surface structure part according to claim 7, which is characterized in that be in step d)
The molar ratio of silicon powder and silicon monoxide is 0.5~3, and sintering temperature is 1300 DEG C~1550 DEG C, 1~6h of sintering time.
9. the preparation method of silicified wood ceramics surface structure part according to claim 8, which is characterized in that be in step d)
The molar ratio of silicon powder and silicon monoxide is 0.7~1.5, and sintering temperature is 1350 DEG C~1450 DEG C, 2~4h of sintering time.
10. a kind of mobile phone backboard, it is characterised in that after timber is processed into hemizygous closed structure, use any of claim 1~9
The preparation method of claim is prepared.
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