CN109320072A - A kind of high alumina low calcium can chemical intensification treatment glass - Google Patents
A kind of high alumina low calcium can chemical intensification treatment glass Download PDFInfo
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- CN109320072A CN109320072A CN201811387152.6A CN201811387152A CN109320072A CN 109320072 A CN109320072 A CN 109320072A CN 201811387152 A CN201811387152 A CN 201811387152A CN 109320072 A CN109320072 A CN 109320072A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
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Abstract
The present invention relates to glass and glass reinforced field of material technology, and in particular to it is a kind of can chemical intensification treatment glass, by percentage to the quality, the glass and ceramics composition include: SiO2: 50%~70%；Al2O3: 12%~25%；Na2O:8%~18%；P2O5: 1%~8%；B2O3: 0%~5%；CaO:0.01%~5%；MgO:0%~5%；ZnO:0%~5%；Li2O:0%~5%；SnO2: 0%~1%；The present invention by introducing P in glass2O5, CaO ingredient so that glass is generated split-phase effect, and pass through Al2O3And P2O5Composition improves the reinforcing performance of glass, so that obtaining has chemically toughened glass, chemically toughened glass is made to have high surface Vickers hardness number.
Description
Technical field
The present invention relates to glass and glass reinforced field of material technology, more specifically to a kind of split-phase glass and glass
Composition, the split-phase glass can carry out chemical intensification treatment.
Background technique
Glass material belongs to fragile material, when glass material receives external forces impact or friction, can not mould
Property deformation and cause damaged or scratch, therefore the mechanical performance of glass surface needs to improve.Chemically enhancing glass, which will mainly pass through, to be contained
The glass material of alkali metal ion is immersed in nitrate solution of 350 DEG C~450 DEG C of the molten state containing sodium or potassium, in hot conditions
Under, alkali-containing glass Ionic Radius is compared with small ion alkali metal ion (Na+And Li+) and the larger ion of nitric acid fused salt Ionic Radius
(K+And Na+) phase double replacement, such as Na in glass occurs+With K in fused salt+Or Li in glass+With Na in fused salt+Generation is mutually set
It changes, to remain one layer in glass surface there is surface compression stress (Compressive Stress, abbreviation CS) and compression to answer
The tempering layer glass of power layer depth (Depth of Layer, abbreviation DOL).After glass carries out chemical tempering processing, glass surface
State change brings the mechanical property of glass to be greatly improved, such as glass surface Vickers hardness number improve, scratch resistance and
Shock resistance improves.By tempering, treated that glass material is widely used in consumer electronics touch-control flat display field is contour
Intensity is shown in shell protection materials.Current more and more mobile electronic equipments (such as mobile phone or wrist-watch) are to the surface of material
Mechanical property proposes more rigors, has been attempted in recent years using materials such as sapphire material, zirconia ceramics and devitrified glasses
Material carrys out gradually substituted chemistry strengthened glass, but above-mentioned material has the shortcomings that manufacture difficulty and cost, and there is presently no big faces
Product uses.Therefore a kind of chemically toughened glass with good surface characteristic is needed to meet the market demand.
It seldom sees at present and high Al is handled using chemical tempering2O3Research and the report of low CaO split-phase glass and glass.
Patent CN104837783A provides the manufacturing method and split-phase glass of split-phase glass, Al in the glass2O3Content
< 10% can carry out chemical strengthening, but too low Al2O3Cause glass surface mechanical property poor.CN104254501B offerization
Learn the manufacturing method of strengthened glass, Al in the glass and the glass2O3< 10wt%, MgO > 5wt% causes surface mechanical special
Property is poor.
Wang Cheng chance etc. is published in emulsion opal glass (four) " glass and enamel " .1998, and volume 26 (the 5th phase) is introduced phosphoric acid cream
Turbid glass, is mainly precipitated phosphatic crystal grain in glass basic ingredient and milkiness, ideal phosphoric acid crystal grain should be coccoid
Distribution.But all emulsion opal glass ingredients are all based on middle Al in document2O3Content is below 12wt% and the emulsion opal glass that obtains,
Thus document is not studied and is illustrated to emulsion opal glass ion-exchange effect and mechanical performance.
Patent CN102249540B provides a kind of Na2O-CaO-SiO2Emulsion opal glass, Al in the glass2O3< 2wt%, because
This described glass ion switching performance is poor, thus glass machinery performance is unable to get and is obviously improved.
CN105967515A provides a kind of ultra-thin emulsion opal glass and preparation method thereof, Al in the glass2O3Content <
3wt%, this described glass ion switching performance is poor, thus glass machinery performance is unable to get and is obviously improved.
Summary of the invention
It is an object of the invention to provide the split-phase glass that one kind can carry out chemical intensification treatment.The present invention by drawing in glass
Enter P2O5、CaO、MgO、Li2O ingredient makes glass generate split-phase effect, and passes through Al2O3And P2O5Composition improves the reinforcing of glass
Can, so that obtaining has chemically toughened glass.
One aspect of the present invention provides a kind of high alumina low calcium split-phase glass, and by percentage to the quality, the composition includes:
SiO2；Na2O；CaO；P2O5；Wherein, Al2O3>=12%, and Al2O3/(P2O5+ CaO) > 2.
Another aspect of the present invention provide a kind of high alumina low calcium can chemical intensification treatment split-phase glass, with mass percent
Meter, the glass composition include:
SiO2: 50%~70 %；
Al2O3: the % of 12 %~25；
Na2The % of O:8 %~18；
P2O5: 1%~8%；
B2O3: the % of 0 %~5；
The % of CaO:0.01 %~5；
The % of MgO:0 %~5；
The % of ZnO:0 %~5；
Li2The % of O:0 %~5；
SnO2: 0%~1%；
Al2O3/(P2O5+ CaO) > 2
The sum of total mass fraction is 100%.
Wherein, the glass surface compression stress value >=500MPa；Compressive stress layers >=20 μm.
Can chemical intensification treatment split-phase glass and glass reinforcing after glass surface Vickers hardness >=650MPa.
SiO2: its major glass formed body belongs to one of essential component, and the main composition netted main structure of glass assigns
The preferable glass structure stability of glass, chemical stability, mechanical performance and processability.SiO in the present invention2Concentration is at least
50wt%, more preferably at least 55wt%；But high SiO in glass2Concentration reduces the split-phase and crystallization ability of glass, while keeping glass molten
Change temperature to improve, occurs the defect of such as a large amount of minute bubbles so as to cause glass, in addition, high SiO2Concentration is tended to chemical steel
Change has an adverse effect, thus SiO2Less than 70wt%, more preferably preferably smaller than 65wt%.
Al2O3: for one of essential component, belong to network intermediate composition.In high-alkalinity glass ingredient, alkali ion
To Al3+Ion carries out charge balance, so that most aluminium oxide is tended to glass aluminum-oxygen tetrahedron, constitutes the netted main knot of glass
Structure, to improve stability, glass and mechanical performance.Al2O3The aluminum-oxygen tetrahedron formed in glass volume ratio silicon in glass
Oxygen tetrahedron volume is big, and glass volume expands, to reduce the density of glass, provides for glass in ion exchange process
Glass compaction stress layer depth is improved, in addition, Al in glass in interchange channel2O3Concentration is to its inhibiting effect of glass phase-separating, it is ensured that glass
Glass keeps the stability of high transmittance and the structure of maintenance split-phase glass, thus Al in glass in phase process2O3Concentration is at least
12wt%, more preferable 15wt%；But it crosses and belongs to pole refractory oxides, can quickly improve high temperature viscosity of glass, cause glass clarifying
It is homogenized difficulty to increase, the air blister defect concentration in glass sharply increases, therefore Al in glass2O3Concentration is less than about 25wt%, more
It is preferred that 23wt%.
Na in glass2O is one of essential component, the Na of glass middle and high concentration2O, so that containing enough Na in glass+
K+ ion swaps in ion, with potassium nitrate fused salt, to generate high compression stress in glass surface.In addition, Na2O it mentions
For a large amount of free oxygen sources, destruction is risen to glass silica network structural body, the viscosity of glass is substantially reduced, facilitates glass
Fusing and clarification, therefore, Na in the present invention2O concentration is not less than 8wt%, more desirably not less than 10wt%.But Na2O excessive concentration, will
Chemical durability of glass is set to deteriorate and be difficult to obtain the glass with high surface strength, therefore Na in glass2The control of O concentration is small
In 18wt%, more preferably less than 16wt%.
Li2O: belong to network outer body composition, can quickly reduce glass melting viscosity, promote glass quickly carry out fusing with it is clear
Clearly；Contain high concentration Li in glass simultaneously+Ion is that glass can be carried out Na+Ion and Li+Ion exchange provides condition, thus energy
It is quickly obtained high compression stress layer depth.
K2O: K in glass in the present invention2O belongs to functionality, K2O can improve glass melting and clarifying effect；Simultaneously
High K2O concentration leads to the reduction of chemically toughened glass surface compression stress but compressive stress layers improve；But high K in glass2O concentration is led
Cause glass surface chemistry stability degradation.Therefore, K in glass of the invention2O concentration is less than 5wt%, more preferable K2O concentration is less than
3%。
B2O3: B in glass2O3At Network former oxide is belonged to, glass viscosity can be reduced and be conducive to produce；In addition,
B2O3There is promotion and stabilization to glass phase-separating in the present invention；Introduce high concentration B2O3There are oxygen during high temperature melting
Compound volatilization phenomenon, is unfavorable for glass ingredient and stablizes, but high B2O3Concentration is unfavorable for chemically toughened glass and obtains high compression stress
With high stress layer depth, therefore by B in the present invention2O3Concentration is less than 5wt%, more preferable B2O3Concentration is 3wt%.
P2O5: belong to one of glass neccessary composition, P in the present invention2O5Belong to glass former ingredient, with [PO4] four sides
Body is mutually interconnected into network, but P2O5The network structure of formation belongs to stratiform, and interlayer is connected with each other by Van der Waals force, makes glass web
Network structure is in rarefaction, and network gap becomes larger, and is conducive to the diffusion of glass intermediate ion, to chemical strengthening facilitation；P simultaneously2O5
To glass phase-separating facilitation.But excessive concentrations P2O5Cause melting fusing volatilization serious, and the chemical stability of glass is deteriorated,
It also results in glass and excessive split-phase occurs and decrease in transmission.Therefore by P in the present invention2O5Concentration is limited in 1wt%~8wt%, excellent
Select P2O5Concentration is in 2wt%~6wt%.
CaO: belong to glass in the present invention and belong to one of neccessary composition, belong to bivalent metal oxide, be glass web
Network ectosome ingredient plays destruction to glass network structure, reduces glass melting temperature, be good fluxing agent, be conducive to clear
Clearly；CaO promotes glass phase-separating effect simultaneously, in glass and P2O5Calcium phosphate crystal grain is precipitated, but excessively high CaO concentration promotes glass
Excessive split-phase, causes glass transmission to reduce.Ca in glass2+Na in ionic radius (0.099nm) and glass+Radius
(0.095nm) is close, and Ca2+Field strength ratio Na+Greatly, therefore in glass sodium ion is mobile will receive Ca2+Limitation, to reduce glass
Glass chemical strengthening efficiency, and CaO excessive concentration in glass, will lead to glass embrittlement.Therefore CaO content is preferred in the present invention
0.01wt%~5wt%, more preferable 1%~3wt%.
MgO: belonging to bivalent metal oxide, is glass network ectosome ingredient, plays destruction to glass network structure,
Glass melting temperature is reduced, is conducive to clarify；To its facilitation of glass phase-separating.And excessively high MgO concentration forms gahnite
(MgAl2O4), cause glass serious split-phase and crystallization occur, leads to glass machinery performance and decrease in transmission.Therefore MgO is dense
Degree is limited in the wt% of 0wt%~5, preferably 1 wt %~3wt %.
ZnO: in high basic metal oxide silicate glass, Zn2+There are hexa-coordinate [ZnO6] and four-coordination [ZnO4] shape
State, wherein hexa-coordinate [ZnO6] structure is comparatively dense, and four-coordination [ZnO4] structure is more loose, four-coordination quantity is with alkali metal
Oxide increases and increases.As four-coordination [ZnO4] content it is more when, glass network is more loose, is conducive to glass intermediate ion
(Na+) migration, thus improve glass ion exchange layer depth, ZnO content to improve glass ion exchange efficiency, exchange depth and
Improving glass surface intensity has positive effect, but the ZnO of excessive concentrations tends to form gahnite (ZnAl2O4) or silicic acid
Zinc (Zn2SiO4), lead to the excessive split-phase of glass.Therefore ZnO concentration is limited in 0wt%~5wt% in the present invention, preferably 1wt %~
3wt%。
By introducing suitable P in the present invention2O5, CaO concentration generate split-phase glass in glass, form crystal phase, such as Fig. 2,
Phase separation structure is generated in glass and is divided into two kinds, and one is the isolated drop-wise structures with dispersion and a kind of three-dimensional space to be connected with each other
Connectivity structure.Can measuring by scanning electron microscopic observation for drop-wise structure split-phase is wherein isolated, as shown in Figure 2.In the present invention
It is preferred that having the isolated drop-wise structure split-phase of dispersion, while in order to improve glass tempering effect, Al should be limited2O3/(P2O5+
CaO) >=2, but split-phase degree needs to control, because of the excessive transmissivity that will affect glass of split-phase.
Remarkable advantage of the invention is:
(1) present invention by introducing suitable P in glass2O5, CaO ingredient so that glass is generated split-phase effect, and pass through Al2O3
And P2O5Composition improves the reinforcing performance of glass, so that obtaining has chemically toughened glass, chemically toughened glass is made to have high table
Face Vickers hardness number.
(2) for glass 1mm thickness of the present invention is in 380nm~780nm wave-length coverage, the average transmittance of the glass
At least 50% or more, the strengthened glass surface compression stress value >=500MPa being prepared；Compressive stress layers >=20 μm；Strengthen glass
Glass surface Vickers hardness number >=650MPa.
Detailed description of the invention
Fig. 1 is the XRD analysis map of embodiment 2；
Fig. 2 is the SEM microgram of embodiment 2.
Specific embodiment
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
The specific embodiment of the invention is as shown in Table 1, according to the material purities such as quartz sand, aluminium oxide, sodium carbonate and moisture content into
Row weighs, and carries out uniformly mixing and obtains uniform ingredient；Then batch is transferred to about 800ml platinum crucible from plastic bottle
In, platinum crucible is placed in Si-Mo rod high temperature furnace, is gradually heated to 1550 DEG C~1650 DEG C, holds temperature 2~6 hours, passes through height
Temperature stirs and holds temperature and accelerates glass blister discharge and be homogenized glass metal.After melting, molten liquid is poured into heat-resistance stainless steel
Mold is formed, and is then taken out glass blocks and is moved into 600 DEG C~630 DEG C heat treatments in 2 hours of progress in box-annealing furnace, with
570 DEG C are down to the rate less than 1 DEG C/minute afterwards, cooled to room temperature.Glass blocks progress cutting and grinding is prepared into and meets phase
Close test non-sample.To obtain more stable measurement result, the cooperation raw material of chemical grade should be selected.
Wherein physical property symbol and measurement method are defined as follows:
The physical property of glass sample is as shown in Table 1.Shown in it defines and is explained as follows:
A. transmissivity: being finished into 1.00 ± 0.05mm thickness for sheet glass upper and lower surface, is divided light using Shimadzu UV, visible light
Degree meter measurement 350nm~780nm transmissivity, and calculate 380nm~780nm average transmittance.
B. CS: surface compression stress Compressive Stress referred to as, that is, uses Zhe Yuan Industrial Co., Ltd of Japan
FSM-6000LE surface stress meter is tested.
C. DOL: surface compression stressor layers Depth of Layer abbreviation, using Japanese Zhe Yuan Industrial Co., Ltd FSM-
6000LE surface stress meter is tested.
D. vickers hardness hv: by glass sample after reinforcing, according to GB/T4340.3-2012, " metal material Vickers hardness is real
Test " standard requirements using Beijing when instead of peak Vickers measure, test condition are as follows: loading force 200g, load time be
15s。
The each embodiment sample of table one and physical property
Claims (10)
1. a kind of high alumina low calcium split-phase glass, which is characterized in that by percentage to the quality, the composition includes: SiO2；Na2O；
CaO；P2O5；Wherein, Al2O3>=12%, and Al2O3/(P2O5+ CaO) > 2.
2. a kind of high alumina low calcium split-phase glass as described in claim 1, which is characterized in that the glass 1mm thickness exists
For in 380nm~780nm wave-length coverage, the average transmittance of the glass at least 50% or more.
3. a kind of high alumina low calcium split-phase glass as described in claim 1, which is characterized in that the glass 1mm thickness exists
For in 380nm~780nm wave-length coverage, the average transmittance of the glass at least 60% or more.
4. a kind of high alumina low calcium split-phase glass as described in claim 1, which is characterized in that the glass is using step chemistry
Reinforcing or multi-step chemical intensive treatment.
5. such as a kind of described in any item high alumina low calcium split-phase glass of claim 1 ~ 4, which is characterized in that strengthened glass surface
Vickers hardness number >=650MPa.
6. such as a kind of described in any item high alumina low calcium split-phase glass of claim 1 ~ 4, which is characterized in that strengthened glass surface
Vickers hardness number >=680MPa.
7. a kind of high alumina low calcium can chemical intensification treatment split-phase glass, which is characterized in that by percentage to the quality, the glass
Composition includes:
SiO2: 50%~75 %；
Al2O3: the % of 12 %~25；
Na2The % of O:8 %~18；
P2O5: 1%~8%；
B2O3: the % of 0 %~5；
The % of CaO:0.01 %~5；
The % of MgO:0 %~5；
The % of ZnO:0 %~5；
Li2The % of O:0 %~5；
SnO2: 0%~1%；
The sum of total mass fraction is 100%；
Wherein, the glass surface compression stress value >=500MPa；Compressive stress layers >=20 μm.
8. high alumina low calcium as claimed in claim 7 can chemical intensification treatment split-phase glass, which is characterized in that wherein Al2O3/
(P2O5+ CaO) > 2.
9. as any one of claim 7 ~ 8 high alumina low calcium can chemical intensification treatment split-phase glass, which is characterized in that strengthen
Glass surface Vickers hardness number >=650MPa.
10. as any one of claim 7 ~ 8 high alumina low calcium can chemical intensification treatment split-phase glass, which is characterized in that it is strong
Change glass surface Vickers hardness number >=680MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111170634A (en) * | 2020-01-10 | 2020-05-19 | 浙江大学 | High-alumina phosphosilicate glass suitable for chemical strengthening and chemically toughened glass |
| CN113149428A (en) * | 2021-04-30 | 2021-07-23 | 科立视材料科技有限公司 | High-alumina glass, high-alumina toughened glass and preparation method thereof |
| CN113264676A (en) * | 2021-06-15 | 2021-08-17 | 武汉理工大学 | Chemically strengthened phase-separated glass and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111170634A (en) * | 2020-01-10 | 2020-05-19 | 浙江大学 | High-alumina phosphosilicate glass suitable for chemical strengthening and chemically toughened glass |
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| CN113264676A (en) * | 2021-06-15 | 2021-08-17 | 武汉理工大学 | Chemically strengthened phase-separated glass and manufacturing method thereof |
| CN113264676B (en) * | 2021-06-15 | 2023-02-17 | 武汉理工大学 | Chemically strengthened phase-separated glass and manufacturing method thereof |
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