CN103524042A - Environment-friendly type high-transmission high-refractivity crystalline glass and preparation method thereof - Google Patents
Environment-friendly type high-transmission high-refractivity crystalline glass and preparation method thereof Download PDFInfo
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- CN103524042A CN103524042A CN201310436184.1A CN201310436184A CN103524042A CN 103524042 A CN103524042 A CN 103524042A CN 201310436184 A CN201310436184 A CN 201310436184A CN 103524042 A CN103524042 A CN 103524042A
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Abstract
The invention discloses environment-friendly type high-transmission high-refractivity crystalline glass and a preparation method thereof. The crystalline glass comprises the following components in percent by mass: 32%-55% of SiO2, 8%-20% of TiO2, 12%-19% of BaO, 0%-4% of K2O, 5%-15% of Na2O, 1%-5% of CaO, 4%-11% of ZnO, 0.2%-2% of Al2O3, 0.2%-0.8% of Sb2O3, 0.005%-0.2% of Er2O3 and 0.005%-0.5% of Nd2O3. The crystalline glass disclosed by the invention does not contain hazardous substances, such as lead, arsenic and fluorine, is not added with rear-earth oxides dear in price, but is excellent in optical performance, and has refractivity of 1.60-1.72, an abbe number of 30-40 and visible light transmission of 89%-92%. The crystalline glass has lower transformation temperature characteristic, and excellent chemical stability and mechanical performance, and is suitable for various forming processes.
Description
Technical field
The present invention relates to the high high refraction crystal glass and preparation method thereof thoroughly of a kind of environment-friendly type, particularly harmful oxide compound, transparency and the specific refractory power such as a kind of not leaded and arsenic not second to the plumbous component of height, be particularly suitable for crystal glass of electrofusion technology and preparation method thereof.
Technical background
To be all that lead tolerance is higher just obtain excellent optical property to general crystal glass, a large amount of for decorating and dinnerware, its feature has been good matter double infection, the specific refractory power of light is high, dispersion is large, and temperature of fusion is low etc., and because plumbous oxide content is high, its temperature of fusion is low, and the content of PbO is by mass percentage between 24-40% conventionally.
But containing lead crystal glass, owing to there being higher lead tolerance, and in use there will be stripping problem, affected HUMAN HEALTH, in addition, the volatilization of lead crystal glass in the process of founding enters after atmosphere by human body suction body and cause various diseases.Along with the continuous progress of science and technology and the enhancing of environmental consciousness, plumbous to the murder by poisoning of human body and the pollution to environment, more and more cause the attention of all sectors of society, unleaded is the inexorable trend of following production high refractive index crystal glass, Ta Dui entire society, the world and even whole terrestrial ecosystem are all to have the major issue that very important practical significance and the strategic importance ，Shi world are harmonious, sustainable development must face and consider.
For Lead contamination problem, European Union etc. have stipulated from 1 day July in 2007, and the objectionable impuritiess such as leaded in the electronics of importing and exporting, mercury are strictly limited, and content should be lower than 10
-9level, Canada Safety Council advises that baby, children do not use containing lead crystal glass vessel.
China goes back at present some glasswork and adopts plumbous oxide to produce crystal glass, in order to control the stripping quantity of plumbous oxide, China has also formulated relevant national standard to plumbous stripping quantity, as regulation small vessels lead release is less than 1.5mg/L, large container is less than 0.75mg/L, and the crystal glass vessel lead release of storage tank class is lower than 0.5 mg/L.
Unleaded high refraction crystal glass be by the lead element in crystal glass be replaced by pollution-free, without other elements of stripping problem, make the glass of making except possessing all characteristics of lead crystal glass, the harmful elements such as not leaded, arsenic, workman's health in production process is guaranteed, more friendly and its moulding is carried out to creative design to environment.
Chinese patent CN 101215084A discloses a kind of leadless crystal glass and has formed, and this crystal glass has higher specific refractory power and transmitance, and specific refractory power, between 1.54-1.61, solved plumbous pollution problem, but it has added KHF
2, introduced F, also be there is to pollution problem in environment, it does not add raising glass specific refractory power and the close BaO of glass in addition, and this matter double infection that crystal glass is required is disadvantageous.
Summary of the invention
The object of the invention is to for still take in the market the crystal glass of high lead content as main, and for using fluorochemical and expensive oxide compound as Nb in leadless crystal glass
2o
5, Ta
2o
5deng deficiency, provide a kind of environment-friendly type not leaded and any harmful oxide compound high high refraction crystal glass thoroughly, its specific refractory power is between 1.60-1.72, visible light transmissivity, between 89-92%, has that color and luster is pure, glass melting temperature is low, chemical stability is good and be easy to the characteristics such as polishing processing.
The present invention also provides the preparation method of above-mentioned crystal glass.
Glass ingredient all produces great impact to the function of glass material or product, character and cost.Glass ingredient and production technique substantial connection, assign to select production technique according to the one-tenth of design conventionally, and Glass Composition Design is improper, causes fusing difficulty, and the defects such as calculus, striped, bubble occur while founding, and in actual production, happens occasionally.Also have, Glass Composition Design must be considered processing performance needs.Conventionally make to design glass ingredient reach be easy to fusing, meet the operational requirements such as shaping, processing and annealing.Finally, when design mix, must consider quality stability and a large amount of supply problem of raw material.
In the present invention, use TiO
2, BaO, ZnO replace PbO, using TiO
2the specific refractory power in time and dispersion increase; While using BaO, the density of glass and specific refractory power increase; While using ZnO, the specific refractory power of glass improves, and the gloss of glass is soft, and adjusts the material property of glass, makes it be easy to found and moulding, uses the CaO(1-5% of appropriate amount), control the material property of glass, be convenient to drawing and the press forming of glass.
The glass composition the present invention relates to is suitable for the preparation technologies such as compacting, float glass process, calendering, overflow, horizontal drawing.
Particularly, the technical solution used in the present invention:
Technical scheme one:
A high high refraction crystal glass thoroughly, comprises following component by weight percentage: SiO
232-55%, TiO
28-20%, BaO 12-19%, K
2o 0-4%, Na
2o 5-15%, CaO 1-5%, ZnO 4-11%, Sb
2o
30.2-0.8%, Al
2o
30.2-2%, Er
2o
30.005-0.2%, Nd
2o
30.005-0.5%.
Wherein BaO is with 5% use Ba (NO of its content
3)
2introduce, all the other are introduced with corresponding carbonate or oxide form.
In said components, SiO
2be important network former, with the structural component of silicon-oxy tetrahedron, form irregular contiguous network, become the skeleton of glass.It not only can form glass, and can improve physical strength, chemical stability, thermostability of glass etc., but it is again more infusibilized material, so SiO
2content has its optimum value.If content cannot obtain this effect fully lower than 30%, the poor chemical stability of glass, quality can not be guaranteed.On the other hand, if content surpasses 60%, the temperature of fusion of glass is high, and viscosity rises, and is difficult to make glass to homogenize.So SiO of the present invention
2content preferably 32～55%.
Al
2o
3be intermediate oxide, energy participation network, plays network and generates body effect, can reduce the crystallization tendency of glass, can improve the viscosity of glass, improves chemical stability, thermostability, physical strength and the specific refractory power of glass.On the other hand, because aluminum oxide compares infusibility, it is large that hardness becomes, and affects founding and polishing processing of glass, so Al of the present invention
2o
3the preferred 0.2-2% of content.
K
2o and Na
2o is network modifying oxide, after introducing, can make silicon-oxy tetrahedron ［ SiO
4formed network is lax, fracture, thereby SiO solved
2infusibilized problem, can be used as fusing assistant, and glass melting temperature is declined, and preferred mass mark is more than 10%.When potassium oxide and sodium oxide total amount are when too low, cause glass to melt difficulty; When total amount is too high, the chemical stability variation of glass.Therefore potassium oxide and sodium oxide should have suitable content, preferred K in the present invention
2o 0-4%, Na
2o 5-15%.
TiO
2have the effect that increases glass refraction, also can increase the dispersion of glass, be to substitute the main oxides of PbO and essential in the present invention.TiO
2content less than 8% time, the specific refractory power of glass does not reach requirement; If surpass 20%, can make glass coloring, owing to making the yellow tendency of glass strengthen to ultraviolet strong absorption, while TiO
2can make again the painted enhancing of Fe in glass, this is disadvantageous to focusing on transparency and the pure crystal glass of color and luster.
BaO substitutes the main oxides of PbO and essential in the present invention, have the effect that increases glass refraction and glass density, and less than 12% can not reach density 2.9g/cm
3target, BaO surpasses 19%, the deaeration of glass in melting process is difficult to carry out, and the erosion aggravation to kiln refractory materials, the melting difficulty that becomes, glass defect increases, degradation is difficult to arrive high-quality crystal glass.
CaO has the effect that reduces glass high temperature viscosity and increase glass low-temperature viscosity, and in the present invention, for the curing speed in the range of working temperature of glass is accelerated, glass material property lengthens, and CaO content is better at 1-5%.
ZnO substitutes the main oxides of PbO and essential in the present invention, have the effect that increases glass refraction, ZnO can not make glass hard (HRC65Yi Shang) become large simultaneously, can improve chemical stability and the thermostability of glass, the viscosity curve of glass is become gently, be conducive to glass and form operation.The content of ZnO of the present invention is better in 4-11% effect.
Sb
2o
3be mainly the finings use as low temperature lower-glass, if do not added in glass, can be covered with a large amount of micro-bubbles, As
2o
3can play same effect, but As
2o
3poisonous being prohibited from using, is used a small amount of Sb in the present invention
2o
3just can play good clarification, the present invention simultaneously will coordinate it to use with part nitrate, and effect is good.
Er
2o
3and Nd
2o
3two kinds of rare earth oxides are used mainly as glassmaker's soap, use trace just can play good decolorizing effect, can increase transparency and the glossiness of glass, consumption too much can make glass coloring on the contrary, according to crystal glass of the present invention, form, both are respectively Er by consumption
2o
30.005-0.2%, Nd
2o
30.005-0.5%, too much makes glass coloring, the very few decolorizing effect that do not have.
Technical scheme two:
The preparation method of described crystal glass, its step is as follows:
(1) frit designing is accurately weighed and mixed;
(2) raw material mixing is added to platinum crucible stove at 1200 ℃, by the heat-up rate of 5 ℃/min, rise to 1400 ℃ of insulation 4-6h and found;
(3) glass melting is cooled to 1300 ℃ of constant temperature 0.5h, pours forming mould moulding into, move to that to close stove after the 2h that anneals in 500 ℃ of annealing furnaces cooling.
Wherein the melting method of step (2) also can carry out except platinum crucible stove in electric furnace kiln or flame kiln, and in step (3), forming method is applicable to the preparation technologies such as compacting, float glass process, calendering, overflow, horizontal drawing.
The glass that the present invention relates to forms when guaranteeing the high transmitance of glass makes specific refractory power reach 1.60-1.72, on market, the crystal glass of selling does not all reach this value, discoloring agent consumption is less just can reach the pure effect of color and luster and decolouring is stable, and product has excellent optical property; The objectionable impurities such as plumbous and arsenic oxide arsenoxide and fluorine of oxygen-freeization in composition, production process environmental protection, product does not have harmful substances stripping problem.
Embodiment
Embodiment mono-:
The quality group of the present embodiment glass becomes: SiO
2: 36.7%, Al
2o
3: 0.45%, TiO
2: 15.9%, CaO:1.30%, BaO:19 %(wherein BaO 5% by Ba (NO
3)
2introduce, all the other are by BaCO
3introducing), K
2o:1.5%, Na
2o:14.5%, ZnO:10%, Sb
2o
3: 0.2%, Er
2o
3: 0.05%, Nd
2o
3: 0.4%.
The preparation method of the present embodiment glass is as follows:
(1) frit of the composition by designing is accurately weighed and mixed;
(2) at 1200 ℃, add platinum crucible to rise to 1400 ℃ of insulation 4-6h by 5 ℃/min heat-up rate the glass batch mixing;
(3) glass melting described in (2) is cooled to 1300 ℃ of constant temperature 0.5h, pours forming mould moulding into, move to that to close stove after the 2h that anneals in 500 ℃ of annealing furnaces cooling;
(4) glass cutting (3) being obtained becomes to require sample grinding and polishing to process, and measures density, specific refractory power, transmitance, the water tolerance of glass.Glass properties: density 3.56g/cm
3, specific refractory power 1.69, transmitance 89.5%, 2 grades of water tolerance.
Embodiment bis-:
The quality group of the present embodiment glass becomes: SiO
2: 40.7%, Al
2o
3: 1.2%, TiO
2: 14.9%, CaO:4.30%, BaO:14 %(wherein BaO 5% by Ba (NO
3)
2introduce, all the other are by BaCO
3introducing), K
2o:3.9%, Na
2o:11.06%, ZnO:9 %, Sb
2o
3: 0.7%, Er
2o
3: 0.04%, Nd
2o
3: 0.2%.
The preparation method of the present embodiment glass is as follows:
(1) frit of the composition by designing is accurately weighed and mixed;
(2) at 1200 ℃, add platinum crucible to rise to 1400 ℃ of insulation 4-6h by 5 ℃/min heat-up rate the glass batch mixing;
(3) glass melting described in (2) is cooled to 1300 ℃ of constant temperature 0.5h, pours forming mould moulding into, move to that to close stove after the 2h that anneals in 500 ℃ of annealing furnaces cooling;
(4) glass cutting (3) being obtained becomes to require sample grinding and polishing to process, and measures density, specific refractory power, transmitance, the water tolerance of glass.Glass properties: density 3.42g/cm
3, specific refractory power 1.67, transmitance 90.2%, 2 grades of water tolerance.
Embodiment tri-:
The quality group of the present embodiment glass becomes: SiO
2: 50.7%, Al
2o
3: 0.55%, TiO
2: 9.9%, CaO:3.78%, BaO:14.7 %(wherein BaO 5% by Ba (NO
3)
2introduce, all the other are by BaCO
3introducing), K
2o:3.5%, Na
2o:12.5%, ZnO:4 %, Sb
2o
3: 0.2%, Er
2o
3: 0.02%, Nd
2o
3: 0.15%.
The preparation method of the present embodiment glass is as follows:
(1) frit of the composition by designing is accurately weighed and mixed;
(2) at 1200 ℃, add platinum crucible to rise to 1400 ℃ of insulation 4-6h by 5 ℃/min heat-up rate the glass batch mixing;
(3) glass melting described in (2) is cooled to 1300 ℃ of constant temperature 0.5h, pours forming mould moulding into, move to that to close stove after the 2h that anneals in 500 ℃ of annealing furnaces cooling;
(4) glass cutting (3) being obtained becomes to require sample grinding and polishing to process, and measures density, specific refractory power, transmitance, the water tolerance of glass.Glass properties: density 3.17g/cm
3, specific refractory power 1.62, transmitance 91%, 2 grades of water tolerance.
Embodiment tetra-:
The quality group of the present embodiment glass becomes: SiO
2: 55%, Al
2o
3: 0.2%, TiO
2: 9.5%, CaO:4.20%, BaO:13 %(wherein BaO 5% by Ba (NO
3)
2introduce, all the other are by BaCO
3introducing), K
2o:3.0%, Na
2o:10.5%, ZnO:4 %, Sb
2o
3: 0.5%, Er
2o
3: 0.02%, Nd
2o
3: 0.08%.
The preparation method of the present embodiment glass is as follows:
(1) frit of the composition by designing is accurately weighed and mixed;
(2) at 1200 ℃, add platinum crucible to rise to 1400 ℃ of insulation 4-6h by 5 ℃/min heat-up rate the glass batch mixing;
(3) glass melting described in (2) is cooled to 1300 ℃ of constant temperature 0.5h, pours forming mould moulding into, move to that to close stove after the 2h that anneals in 500 ℃ of annealing furnaces cooling;
(4) glass cutting (3) being obtained becomes to require sample grinding and polishing to process, and measures density, specific refractory power, transmitance, the water tolerance of glass.Glass properties: density 3.04g/cm
3, specific refractory power 1.60, transmitance 92 %, 2 grades of water tolerance.
Claims (4)
1. the high high refraction crystal glass thoroughly of environment-friendly type, is characterized in that comprising following component by weight percentage: SiO
232-55%, Al
2o
30.2-2%, TiO
28-20%, BaO 12-19%, K
2o 0-4%, Na
2o 5-15%, CaO 1-5%, ZnO 4-11%, Sb
2o
30.2-0.8%, Er
2o
30.005-0.2%, Nd
2o
30.005-0.5%.
2. crystal glass according to claim 1, described in it is characterized in that wherein BaO with 5% use Ba (NO of its content
3)
2introduce, all the other are introduced with corresponding carbonate or oxide form.
3. crystal glass according to claim 1 and 2, is characterized in that K
2o and Na
2the content sum of O is 9-19%.
4. the preparation method of crystal glass claimed in claim 1, is characterized in that its step is as follows:
(1) frit designing is accurately weighed and mixed;
(2) raw material mixing is added to platinum crucible stove at 1200 ℃, by the heat-up rate of 5 ℃/min, rise to 1400 ℃ of insulation 4-6h and found;
(3) glass melting is cooled to 1300 ℃ of constant temperature 0.5h, pours forming mould moulding into, move to that to close stove after the 2h that anneals in 500 ℃ of annealing furnaces cooling.
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|---|---|---|---|
| CN201310436184.1A CN103524042B (en) | 2013-09-24 | 2013-09-24 | A kind of environment-friendly type height high refraction crystal glass and its preparation method thoroughly |
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| CN103524042B CN103524042B (en) | 2016-06-01 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031460A (en) * | 2014-06-27 | 2014-09-10 | 威远县大禾陶瓷原料有限公司 | Inorganic filler material for transparent lacquer and preparation method thereof |
| CN104445925A (en) * | 2014-12-01 | 2015-03-25 | 河北省沙河玻璃技术研究院 | Ultra-high-refractivity environment-friendly cameo glass and preparation method thereof |
| CN106673460A (en) * | 2017-01-18 | 2017-05-17 | 河北省沙河玻璃技术研究院 | Method for increasing brightness and refractive index of lead-free crystalline glass |
| CN109912195A (en) * | 2019-04-24 | 2019-06-21 | 成都光明光电股份有限公司 | Optical glass, gas preform, optical element and optical instrument |
| CN109942184A (en) * | 2019-04-12 | 2019-06-28 | 和县晶晶玻璃制品有限公司 | A kind of high refraction crystal glass and its production technology |
| CN110255872A (en) * | 2019-06-10 | 2019-09-20 | 成都恒达光学有限公司 | A kind of high light transmission glass tempering technique |
| CN110950532A (en) * | 2020-01-07 | 2020-04-03 | 山东理工大学 | Zirconia-based lead-free crystal glass and preparation method thereof |
| CN110981189A (en) * | 2020-01-08 | 2020-04-10 | 山东理工大学 | Zinc oxide-based lead-free crystal glass and preparation method thereof |
| CN110981191A (en) * | 2020-01-07 | 2020-04-10 | 山东理工大学 | Titanium oxide-based lead-free crystal glass and preparation method thereof |
| CN111018347A (en) * | 2020-01-07 | 2020-04-17 | 山东理工大学 | Lanthanum oxide-based lead-free crystal glass and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031460A (en) * | 2014-06-27 | 2014-09-10 | 威远县大禾陶瓷原料有限公司 | Inorganic filler material for transparent lacquer and preparation method thereof |
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| CN106673460A (en) * | 2017-01-18 | 2017-05-17 | 河北省沙河玻璃技术研究院 | Method for increasing brightness and refractive index of lead-free crystalline glass |
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| CN109912195A (en) * | 2019-04-24 | 2019-06-21 | 成都光明光电股份有限公司 | Optical glass, gas preform, optical element and optical instrument |
| CN109912195B (en) * | 2019-04-24 | 2021-12-07 | 成都光明光电股份有限公司 | Optical glass, glass preform, optical element and optical instrument |
| CN110255872A (en) * | 2019-06-10 | 2019-09-20 | 成都恒达光学有限公司 | A kind of high light transmission glass tempering technique |
| CN110950532A (en) * | 2020-01-07 | 2020-04-03 | 山东理工大学 | Zirconia-based lead-free crystal glass and preparation method thereof |
| CN110981191A (en) * | 2020-01-07 | 2020-04-10 | 山东理工大学 | Titanium oxide-based lead-free crystal glass and preparation method thereof |
| CN111018347A (en) * | 2020-01-07 | 2020-04-17 | 山东理工大学 | Lanthanum oxide-based lead-free crystal glass and preparation method thereof |
| CN110981189A (en) * | 2020-01-08 | 2020-04-10 | 山东理工大学 | Zinc oxide-based lead-free crystal glass and preparation method thereof |
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