CN109809696A - A kind of magnalium silicon spinel devitrified glass - Google Patents
A kind of magnalium silicon spinel devitrified glass Download PDFInfo
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Abstract
A kind of magnalium silicon spinel devitrified glass, by weight percentage its component are as follows: Al2O3 20-45wt%, SiO2 25-60wt%, MgO 8-18wt%, 3 TiO2~0~5wt% of 10wt%, ZrO2,0~3wt% of P2O5,0~2wt% of Li2O, 0~2wt% of Na2O, 0~2wt% of K2O, Sb2O3 0.5-3wt%.This product have the characteristics that it is high-strength, high it is hard, resistance to fall, low bulk, dielectric properties it is superior.
Description
Technical field
The present invention relates to microcrystal glass areas, and in particular to a kind of magnalium silicon spinel devitrified glass and preparation method thereof.
Background technique
Devitrified glass is specific components glass dominated crystallization and a kind of polycrystalline solids material formed, with glass and pottery
The structure feature and performance of porcelain are a kind of novel inorganic nonmetallic materials for developing, having a extensive future.Spinel crystallites
Glass is a kind of using spinelle as the devitrified glass of principal crystalline phase, has lower thermal expansion coefficient, good corrosion resistance, mechanical strength
Height, hardness is very high (Mohs' hardness~8), and wearability is good, good thermal shock, and the excellent equal excellent properties of dielectric properties can be used as electricity
Base board, device outer case, capacitor material, solid state laser etc. have extensively in fields such as mechanical engineering, microelectronics, optical engineering
General application prospect.
Spinel crystallites glass applications have apparent comparative advantages: with zirconium oxide in the rear cover of the signal equipments such as mobile phone
Ceramic rear cover is compared, and spinel crystallites glass surface is bright and clean, the complete dense uniform of structure, is not easy to stain, and technique is relatively easy, produces
Energy is big, cost is relatively low；Compared with high alumina glass back cover, spinel crystallites glass has higher mechanical strength, hardness, resistance to falls
Property, thermal conductivity and more excellent thermal stability and chemical stability etc..Spinel crystallites glass is used into ultra-thin forming technique
The glass-ceramic panel for being made into thickness about 0.7mm just can satisfy under comprehensive screen, wireless charging, 5G signal trend to cell phone rear cover
Harsh thickness, mechanics, calorifics and electrical performance requirements.
Disclosed in patent US5968857 it is a kind of using spinelle as the devitrified glass of principal crystalline phase, with 45~65%SiO2,
14~28%Al2O3,4~13%ZnO, 0~8%MgO, 0~10%TiO2,0~6%ZrO2,0~8%BaO, 0~15%
Cs2O, ZnO+MgO are basic composition, have visible light transmittance up to 85% performance.
Pinckney and Beall in 1997 develops the saturating of SiO2-Al2O3-Li2O-ZnO-MgO system fine grain and Ultra-fine Grained
Bright spinel crystallites glass.Research has shown that TiO2 can make this system glass that split-phase occur, to promote different crystal phase coring.
This devitrified glass chemical stability is good, and heat resistance improves.
Time rosy clouds of dawn etc. is prepared for putting down with 50%SiO2,23%Al2O3,18%ZnO, 3%Li2O, 5%TiO2,1%Sb2O3
Equal crystallite dimension is only 20nm or so Gahnite Transparent Glass-ceramics.Tang Liying etc. is introduced using TiO2, ZrO2 as Nucleating Agent
It can make fluxing agent but also participate in the ZnO (0-4wt%) of spinel crystal structure.Preparation MgO- is heat-treated with " two-step method "
Al2O3-SiO2 system is colourless, transparent glass-ceramics.
CN104478219A with 56~62%SiO2,19~23%Al2O3,6~15%ZnO, 2~6.5%MgO, 2~
6%TiO2,2~7%ZrO2 are basic composition, have obtained the spinel crystallites glass of 30-100nm.
Currently, the inorganic non-metallic material of the signal equipments rear cover such as smart phone is mainly glass and ceramics.Samsung
Galaxy series and apple 2017 new architecture smart phones are all made of glass back cover design.IPone 8 and iPone X is used
5th generation gorilla glass of Corning Incorporated belongs to aluminium silicon tempered glass.It is to be understood that although glass back cover technique at
Ripe, production capacity is greatly, cost is relatively low, but also fairly obvious the shortcomings that glass back cover, poor heat conduction, and intensity and hardness are not enough (not
For family name's hardness lower than 7), frangible easy to crack, crash resistance is weaker, easily leaves expendable large area scar, seriously restricts glass and exists
Application in the signal equipments such as smart phone.Another rear cover material is high technology ceramics, mainly uses zirconia ceramics material at present
Material, beautiful exquisiteness, drop resistant is wear-resisting, hardness is high (Mohs' hardness is only second to sapphire), thermal diffusivity is good, becomes high-end smartphones
Allocation plan.For example the ceramic Premium Edition of millet 6 just uses zirconia ceramics cell phone rear cover.But meanwhile zirconia ceramics rear cover
There is also very high to Zirconium powder performance requirement, production capacity is insufficient and the problems such as at high price；Moreover, zirconia ceramics needs
By processing procedures such as nanometer grade powder preparation, slurry, granulation, molding, sintering, post-processings, process is overflow long and complex, leads to product
Yields is low, seriously affects large-scale promotion application of the ceramic material in the signal equipments such as smart phone.
Relevant report of the spinel crystallites glass for smart phone rear cover is had no at present.Pertinent literature above-mentioned is
Bright zinc-magnesium aluminate devitrified glass, crystal size is between 20-100nm.
Furthermore also fairly obvious the shortcomings that glass back cover, poor heat conduction, not enough (Mohs' hardness is lower than for intensity and hardness
7), frangible easy to crack, crash resistance is weaker, easily leaves expendable large area scar；Zirconia ceramics rear cover exists to zirconium oxide
Powder characteristic requires that very high, production capacity is insufficient and the problems such as at high price；Moreover, zirconia ceramics need to pass through nanometer grade powder
The processing procedures such as preparation, slurry, granulation, molding, sintering, post-processing, process are overflow long and complex, cause the yields of product low, and it
Specific gravity it is larger.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of magnalium silicon spinel devitrified glasses:
A kind of intelligence 5G cell phone rear cover magnalium silicon spinel devitrified glass, by weight percentage its component are as follows:
Al2O320-45wt%, SiO225-60wt%, MgO 8-18wt%, TiO23~10wt%, ZrO20~5wt%, P2O50~
0~2wt% of 3wt%, Li2O, 0~2wt% of Na2O, 0~2wt% of K2O, Sb2O30.5-3wt%.
Preferably, the SiO2 constituent content is 30~45wt%.
Preferably, the Al2O3 constituent content is 30~40wt%, can effectively avoid molding high viscosity and mullite analysis
Brilliant appearance.
Preferably, the MgO constituent content is 10~16wt%.Minimum content needed for MgO is 8wt%, but its content
There is undesirable crystallization when manufacturing process especially melts difficult and molding when more than 17wt%, therefore in 10~16wt%
It is comparatively suitable range.
Preferably, the constituent content of the sum of described Na2O+K2O is 0.5~4wt%.Alkali-Metal Na 2O, K2O additive
Crystallization when effect is fluxing and reduction molding.But since these ingredients will not enter crystal phase but stay in the residual of devitrified glass
In remaining glass phase, excessively high content causes the performance of devitrified glass to be affected, and hinders initial glass to devitrified glass
Transformation.Alkali-Metal Na 2O+K2O and at least 0.2wt%, preferred minimum value 0.5wt%.
Preferably, the Li2O constituent content is 1~2.5%wt%.The effect of Li2O is dual, existing fluxing work
With, and play the role of participating in crystallization, this does not refer to its application in all pertinent literatures.Suitable additional amount is 1~4%
Wt%, it is too low not have fluxing action, it is too high to generate β-quartz solid solution, and then there is best effect within the above range
Fruit.
Preferably, the constituent content of the sum of described TiO2+ZrO2 is 3~12%wt%, and wherein the constituent content of ZrO2 is
1.5~4wt%.
Preferably, the constituent content of P2O5 is 1~3wt%.TiO2, ZrO2, P2O5 are Nucleating Agents, are existed as devitrified glass
The seed of crystal when crystallization.Since the crystallization ability of magnalium silicon spinel devitrified glass is weaker, the amount of the total Nucleating Agent needed
It is higher.
A kind of preparation method of magnalium silicon spinel devitrified glass, includes the following steps:
S1: fused silica crucible is added in the above raw material after evenly mixing, continues S2；
S2: Si-Mo rod hot plate is warming up to 1600~1650 DEG C with 5~10 DEG C/min and keeps the temperature 4~5h, continues S3；
S3: the glass metal melted pours into die for molding, and cooling and demolding is placed on 600 DEG C or so 1~2h of electric furnace annealing,
It is cooled to room temperature later, continues S4；
S4: differential thermal differential analysis (DSC), which is tested, determines crystallization peak temperature Tf, continues S5；
S5: the glass frit after annealing carries out the ultra-thin forming of glass frit, the glass after making annealing using second polishing method
Glass frit is shaped to two sides grinding, polishing continuation S6 after the thin slice of about 0.7~1mm；
S6: the thin sheet glass of polishing is cut into appropriate size, is put into special mold and rises to 800 DEG C of pre- cores with 10 DEG C/min
Change processing 4 hours, crystallization and thermal treatment under crystallization temperature Tf is then risen to certain 10 DEG C/min of heating rate, obtains rear cover shape
The spinel crystallites glassware of shape.
Preferably, a kind of preparation method of magnalium silicon spinel devitrified glass, the step S5 use Buddha's warrior attendant wire cutting skill
Art, the glass frit after making annealing are shaped to two sides grinding, polishing after the thin slice of about 0.7~1mm.
The invention has the following beneficial effects: compared with zirconia ceramics rear cover, spinel crystallites glass table of the invention
Face is bright and clean, structure is complete, dense uniform, is not easy to stain, and technique is relatively easy, production capacity is big, light weight and cost is lower；With glass
Rear cover is compared, and spinel crystallites glass has higher mechanical strength, hardness, resistance to falling property, thermal conductivity and more excellent heat steady
The advantages that qualitative and chemical stability.
Furthermore devitrified glass produced by the invention with glass and ceramics structure feature and performance, mechanical strength with
Hardness is higher, and wherein Mohs' hardness is up to 8.Dielectric properties excellent spinel crystallites glass is used for smart phone rear cover material
Material passes through the key technologies such as the design of spinel crystallites glass composition, spinel crystal phase formation and control, the ultra-thin forming of second polishing
Break through, prepare thickness 0.7mm or less, it is high-strength, high it is hard, resistance to fall, low bulk, the superior magnalium silicon spinel of dielectric properties it is micro-
Crystal glass panel may replace high alumina glass panel and zirconia ceramics panel, for communication equipments rear covers such as smart phones, meet
Great demand and the fast-developing particular/special requirements such as comprehensive screen, wireless charging, 5G communication.
Detailed description of the invention
Fig. 1 is process flow chart.
Fig. 2 is embodiment chart.
Fig. 3 is the XRD diagram of product.
Specific embodiment
Invention is further explained for each embodiment in 1-3 and embodiment chart with reference to the accompanying drawing.
A kind of magnalium silicon spinel devitrified glass is primarily useful for intelligent 5G hand using magnesium aluminate spinel as principal crystalline phase
The ultra-thin white spinel crystallites glass of machine rear cover.Its basic ingredient by SiO2, Al2O3, MgO, TiO2, ZrO2, P2O5 and
Li2O and Na2O or K2O composition, additional clarifying agent Sb2O3.The composition of devitrified glass of the present invention is by weight percentage are as follows:
Al2O320-45wt%, SiO225-60wt%, MgO8-18wt%, TiO23~10wt%, ZrO20~5wt%, P2O50~
0~2wt% of 3wt%, Li2O, Na2O0~2wt%, 0~2wt% of K2O, Sb2O30.5-3wt%.
SiO2, Al2O3, MgO have certain composition range in the devitrified glass that magnesium aluminate spinel is principal crystalline phase.Foundation
The comprehensive analysis of its three-phase diagram and its fusing and principal crystalline phase, SiO2 content is limited in 25~60wt%, it is preferably chosen as 30~
45wt%.In order to avoid the appearance of molding high viscosity and mullite crystallization, 20~45wt% of content of Al2O3 is preferably selected
For 30~40wt%.Minimum content needed for MgO is 8wt%, but is especially melted when its content is more than 17wt% in manufacturing process
There is undesirable crystallization when changing difficult and molding, more appropriate range is between 10~16wt%.
The crystallization when effect of Alkali-Metal Na 2O, K2O additive is fluxing and reduction molding.But not due to these ingredients
Crystal phase can be entered but stayed in the remaining glass phase of devitrified glass, excessively high content causes the performance of devitrified glass by shadow
It rings, and hinders transformation of the initial glass to devitrified glass.Alkali-Metal Na 2O+K2O's and at least 0.2wt%, it is preferably minimum
Value is 0.5wt%.The preferred 3.5wt% of maximum value 4wt%.The effect of Li2O is dual, existing fluxing effect, and has participation
The effect of crystallization, this does not refer to its application in all pertinent literatures.Suitable additional amount is 1~4%wt%, too low
Less than fluxing action, too high to generate β-quartz solid solution, preferred content is 1~2.5%wt%.
TiO2, ZrO2, P2O5 are Nucleating Agents, the seed as devitrified glass crystal in crystallization.Since magnalium silicon tip is brilliant
The crystallization ability of stone devitrified glass is weaker, and the higher TiO2+ZrO2 content of the amount of the total Nucleating Agent needed is 3~12%wt%,
It is preferred that 5~12%wt%.ZrO2 content is in 0~5wt%, preferably 1.5~4wt%.Excessively high ZrO2 content glass melting is difficult,
To guarantee that higher crystallization rate, the minimum content of ZrO2 are 1.5wt%, preferably 2wt%.The content of TiO2 is 3~10wt%
Between, preferably minimum 5wt% is to guarantee quick coring under faster crystallization rate, crystallization when can cause to form higher than 10wt%.
It is preferred that the content of TiO2 is between 5~10wt%.P2O5 is both Nucleating Agent and the fluxing agent of ZrO2, and P2O50~3wt% is excellent
Select 1~3wt%.
By above-mentioned analysis it is found that the composition of devitrified glass optimization is as follows:
Al2O330~40wt%, SiO230~45wt%, 10~16wt% of MgO, TiO25~10wt%, ZrO21.5~
4wt%, P2O51~1~2.5wt% of 3wt%, Li2O, 0~2wt% of Na2O, 0~2wt% of K2O, Sb2O30.5-3wt%,
0.5~3.5wt% of Na2O+K2O, TiO2+ZrO23~12%wt%.
A kind of preparation method of magnalium silicon spinel devitrified glass, includes the following steps:
S1: fused silica crucible is added in the above raw material after evenly mixing, continues S2；
S2: Si-Mo rod hot plate is warming up to 1600~1650 DEG C with 5~10 DEG C/min and keeps the temperature 4~5h, continues S3；
S3: the glass metal melted pours into die for molding, and cooling and demolding is placed on 600 DEG C or so 1~2h of electric furnace annealing,
It is cooled to room temperature later, continues S4；
S4: differential thermal differential analysis (DSC), which is tested, determines crystallization peak temperature Tf, continues S5；
S5: the glass frit after annealing carries out the ultra-thin forming of glass frit using second polishing method, it is preferred to use Buddha's warrior attendant
Line cutting technology, the glass frit after making annealing are shaped to two sides grinding, polishing continuation S6 after the thin slice of about 0.7~1mm；
S6: the thin sheet glass of polishing is cut into appropriate size, is put into special mold and rises to 800 DEG C of pre- cores with 10 DEG C/min
Change processing 4 hours, crystallization and thermal treatment under crystallization temperature Tf is then risen to certain 10 DEG C/min of heating rate, obtains rear cover shape
The spinel crystallites glassware of shape.
Obviously, the above embodiment of the present invention is intended to be merely illustrative of the present example, and not to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no need and unable to give poor example to all embodiments.And these belong to this
The connotation changes and variations that derived from of invention still fall within protection scope of the present invention.
Claims (10)
1. a kind of magnalium silicon spinel devitrified glass, which is characterized in that its component by weight percentage are as follows: Al2O320-
45wt%, SiO225-60wt%, MgO 8-18wt%, TiO23~10wt%, ZrO20~5wt%, P2O50~3wt%,
0~2wt% of Li2O, 0~2wt% of Na2O, 0~2wt% of K2O, Sb2O30.5-3wt%.
2. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the SiO2 constituent content is 30
~45wt%.
3. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the Al2O3 constituent content is
30~40wt%.
4. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the MgO constituent content is 10
~16wt%.
5. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the group of the sum of described Na2O+K2O
Dividing content is 0.5~4wt%.
6. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the Li2O constituent content is 1
~2.5%wt%.
7. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the sum of described TiO2+ZrO2's
Constituent content is 3~12%wt%, and wherein the constituent content of ZrO2 is 1.5~4wt%.
8. magnalium silicon spinel devitrified glass according to claim 1, it is characterised in that: the constituent content of the P2O5 is
1~3wt%.
9. a kind of preparation method of any magnalium silicon spinel devitrified glass of claim 1-8, which is characterized in that including
Following steps:
S1: fused silica crucible is added in the above raw material after evenly mixing, continues S2；
S2: Si-Mo rod hot plate is warming up to 1600~1650 DEG C with 5~10 DEG C/min and keeps the temperature 4~5h, continues S3；
S3: the glass metal melted pours into die for molding, and cooling and demolding is placed on 600 DEG C or so 1~2h of electric furnace annealing, later
It is cooled to room temperature, continues S4；
S4: differential thermal differential analysis (DSC), which is tested, determines crystallization peak temperature Tf, continues S5；
S5: the glass frit after annealing carries out the ultra-thin forming of glass frit using second polishing method, and the glass after making annealing is molten
Two sides grinding, polishing continue S6 after the thin slice that formation of lots is about 0.7~1mm；
S6: the thin sheet glass of polishing is cut into appropriate size, is put into special mold and is risen at 800 DEG C of pre- coring with 10 DEG C/min
Reason 4 hours, then rises to crystallization and thermal treatment under crystallization temperature Tf with certain 10 DEG C/min of heating rate, obtains rear cover shape
Spinel crystallites glassware.
10. a kind of preparation method of magnalium silicon spinel devitrified glass as claimed in claim 9, which is characterized in that the step
S5 uses Buddha's warrior attendant line cutting technology.
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| CN113735450A (en) * | 2021-09-09 | 2021-12-03 | 温州市康尔微晶器皿有限公司 | Transparent high-hardness magnesium-aluminum-silicon microcrystalline glass and preparation method thereof |
| CN113735450B (en) * | 2021-09-09 | 2022-12-20 | 温州市康尔微晶器皿有限公司 | Transparent high-hardness magnesium-aluminum-silicon microcrystalline glass and preparation method thereof |
| WO2023125035A1 (en) * | 2021-12-30 | 2023-07-06 | 重庆鑫景特种玻璃有限公司 | Transparent spinel glass ceramic and preparation method therefor and use thereof |
| EP4299537A4 (en) * | 2021-12-30 | 2024-09-18 | Chongqing Aureavia Hi Tech Glass Co Ltd | Transparent spinel glass ceramic and preparation method therefor and use thereof |
| CN114988863A (en) * | 2022-06-29 | 2022-09-02 | 江苏师范大学 | Method for preparing magnesia-alumina spinel transparent ceramic by amorphous crystallization |
| CN117550800A (en) * | 2022-08-04 | 2024-02-13 | 清远南玻节能新材料有限公司 | Aluminum magnesium glass and preparation method and application thereof |
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