CN105541110A - Glass material for filling emeralds and preparation method of glass material - Google Patents

Glass material for filling emeralds and preparation method of glass material Download PDF

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Publication number
CN105541110A
CN105541110A CN201610116144.2A CN201610116144A CN105541110A CN 105541110 A CN105541110 A CN 105541110A CN 201610116144 A CN201610116144 A CN 201610116144A CN 105541110 A CN105541110 A CN 105541110A
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mol
filling
glass
emerald
crucible
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CN201610116144.2A
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胡静雯
王以群
史凌云
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East China University of Science and Technology
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East China University of Science and Technology
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Priority to CN201610116144.2A priority Critical patent/CN105541110A/en
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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
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
    • C03C3/247—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron containing fluorine and phosphorus

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses lead-free and low-melting-point fluorphosphate glass for filling emeralds. A glass material for filling the emeralds comprises components in mole percentage as follows: 20 mol%-40 mol% of P2O5, 5 mol%-10 mol% of B2O3, 7 mol%-15 mol% of CaF2, 8 mol%-15 mol% of BaF2, 2 mol%-10 mol% of LiF and 30 mol%-50 mol% of NaF; the sum of the mole percentage of the components is 100 mol%. A preparation method comprises the following steps: weighing raw materials according to a formula; fully and evenly mixing the raw materials, and then putting the evenly mixed raw materials in a crucible for presintering for 30-40 min; transferring the presintered raw materials to a crucible at the temperature of 850-1000 DEG C for heat preservation for 30-40 min. The softening temperature of the glass material is as low as 353 DEG C, and the glass material has outstanding acid-resistant and alkali-resistant performance; the preparation process is simple, and operation is easy.

Description

A kind of emerald filling glass material and preparation method thereof
Technical field
The present invention relates to emerald fracture filling glass material, particularly a kind of Unlead low-smelting point fluorphosphate glass material and preparation method thereof.
Background technology
Emerald (Emerald) is internationally recognized chalchihuitl the most expensive and ancient, but its property is crisp, and cranny development enriches, and has had a strong impact on quality and soundness.Hexagonal columnar blank pipe in emerald structure includes a kind of water of constitution of specific type, thermal treatment need lower than 500 DEG C with prevent emerald because of dehydration devitrification.Therefore, some organism cedar oils, sweet oil, Cedrus deoclar (Roxb.) G. Don oil, paraffin and artificial/natural resin are applied to the filling of emerald.But these organic charges exist certain defect, to turn yellow along with the time, aging, natural oils can by thermal evaporation residual yellow spot inner in crack, and resene can come off because collision scraped finish.
For avoiding above-mentioned defect, a kind of novel emerald compaction material needs to be developed.About emerald fracture filling glass material, all there is not bibliographical information both at home and abroad at present.The leaded low melting glass of tradition is replaced by Unlead low-smelting point glass gradually because its contaminative is large, harmful, is mainly divided into the systems such as phosphoric acid salt, borate, bismuthate.Wherein, phosphate-based low melting glass has lower softening temperature, and environmental friendliness, aboundresources, cheap, but most phosphates chemical durability of glass is poor.
The softening temperature of the Unlead low-smelting point fluorphosphate glass material that the present invention studies is low to moderate 353 DEG C, and has excellent chemical stability.
Summary of the invention
The object of this invention is to provide and be a kind ofly applied to the low melting point of emerald fracture filling and unleaded fluorphosphate glass of stable chemical nature and preparation method thereof.
This object is realized by the theme of patent claims.The molar percentage of Unlead low-smelting point fluorphosphate glass of the present invention consists of:
P 2O 5：20-40mol%，
B 2O 3：5-10mol%，
CaF 2:7-15mol%，
BaF 2:8-15mol%，
LiF:2-10mol%，
NaF:30-50mol%，
Said components and be 100mol%,
Wherein, P 2o 5can by primary ammonium phosphate (NH 4h 2pO 4) introduce, B 2o 3by boric acid (H 3bO 3) introduce.
Unlead low-smelting point fluorphosphate glass of the present invention has carried out following steps in preparation process:
First, take raw material by formula, after fully mixing, put into crucible.If with NH 4h 2pO 4for raw material replaces P 2o 5, then first crucible should be moved to pre-burning 30-40min in the retort furnace being warming up to 300 DEG C in advance, discharge to make the ammonia in primary ammonium phosphate.If with P 2o 5for raw material, then direct being transferred to by crucible in the retort furnace of 850-1000 DEG C founds 30-40min; Then, glass metal is placed in the retort furnace that is warming up near second-order transition temperature in copper coin top casting slivering the 3h that anneals, cools to room temperature with the furnace.
The invention has the advantages that:
(1) chemical stability of the Unlead low-smelting point fluorphosphate glass that the present invention relates to is excellent, and without any physicochemical change in basic solution, in the acidic solution of PH=4, weight loss is lower than 4.53E-4mg/cm 2/ day.
(2) softening temperature of the Unlead low-smelting point fluorphosphate glass that the present invention relates to is low to moderate 353 DEG C.
Accompanying drawing explanation
Fig. 1 is the reduced gravity situations of Unlead low-smelting point fluorphosphate glass of the present invention in the synthetic perspiration of PH=4
Fig. 2 is the T of Unlead low-smelting point fluorphosphate glass of the present invention g, T fchange curve
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1:30NaF-7LiF-9BaF 2-7CaF 2-7B 2o 3-40P 2o 5
Preparation method: take primary ammonium phosphate (NH respectively 4h 2pO 4) 18.205g, boric acid (H 3bO 3) 1.713g, barium fluoride (BaF2) 3.122g, Calcium Fluoride (Fluorspan) (CaF2) 1.081, Sodium Fluoride (NaF) 2.492g, lithium fluoride (LiF) 0.359g.The raw material weighed in molar ratio is put into agate mortar grind, pour in corundum crucible pre-burning 30-40min in the retort furnace moving to and be warming up to 300 DEG C in advance after Homogeneous phase mixing into, crucible burned is in advance transferred in the retort furnace of 850-1000 DEG C and founds 30-40min.Finally, anneal glass metal 3h after copper coin top casting slivering at 300-450 DEG C, cools to room temperature with the furnace.Carry out test analysis after glass after annealing is polished into specific dimensions, result as shown in Figure 1 and Figure 2.The weight loss of glass sample in the synthetic perspiration of PH=4 is 4.53E-4mg/cm 2/ day, its T g, T fbe respectively 292 DEG C, 353 DEG C.
Embodiment 2:35NaF-7LiF-9BaF 2-7CaF 2-7B 2o 3-35P 2o 5
Preparation method: take primary ammonium phosphate (NH respectively 4h 2pO 4) 16.758g, boric acid (H 3bO 3) 1.802g, barium fluoride (BaF2) 3.284g, Calcium Fluoride (Fluorspan) (CaF2) 1.137, Sodium Fluoride (NaF) 3.059g, lithium fluoride (LiF) 0.378g.The raw material weighed in molar ratio is put into agate mortar grind, pour in corundum crucible pre-burning 30-40min in the retort furnace moving to and be warming up to 300 DEG C in advance after Homogeneous phase mixing into, crucible burned is in advance transferred in the retort furnace of 850-1000 DEG C and founds 30-40min.Finally, anneal glass metal 3h after copper coin top casting slivering at 300-450 DEG C, cools to room temperature with the furnace.Carry out test analysis after glass after annealing is polished into specific dimensions, result as shown in Figure 1 and Figure 2.The weight loss of glass sample in the synthetic perspiration of PH=4 is 4.13E-4mg/cm 2/ day, its T g, T fbe respectively 328 DEG C, 375 DEG C.
Embodiment 3:40NaF-7LiF-9BaF 2-7CaF 2-7B 2o 3-30P 2o 5
Preparation method: take primary ammonium phosphate (NH respectively 4h 2pO 4) 15.152g, boric acid (H 3bO 3) 1.901g, barium fluoride (BaF2) 3.464g, Calcium Fluoride (Fluorspan) (CaF2) 1.120, Sodium Fluoride (NaF) 3.688g, lithium fluoride (LiF) 0.399g.The raw material weighed in molar ratio is put into agate mortar grind, pour in corundum crucible pre-burning 30-40min in the retort furnace moving to and be warming up to 300 DEG C in advance after Homogeneous phase mixing into, crucible burned is in advance transferred in the retort furnace of 850-1000 DEG C and founds 30-40min.Finally, anneal glass metal 3h after copper coin top casting slivering at 300-450 DEG C, cools to room temperature with the furnace.Carry out test analysis after glass after annealing is polished into specific dimensions, result as shown in Figure 1 and Figure 2.The weight loss of glass sample in the synthetic perspiration of PH=4 is 3.50E-4mg/cm 2/ day, its T g, T fbe respectively 365 DEG C, 409 DEG C.
Embodiment 4:45NaF-7LiF-9BaF 2-7CaF 2-7B 2o 3-25P 2o 5
Preparation method: take primary ammonium phosphate (NH respectively 4h 2pO 4) 13.359g, boric acid (H 3bO 3) 2.011g, barium fluoride (BaF2) 3.665g, Calcium Fluoride (Fluorspan) (CaF2) 1.269, Sodium Fluoride (NaF) 4.389g, lithium fluoride (LiF) 0.422g.The raw material weighed in molar ratio is put into agate mortar grind, pour in corundum crucible pre-burning 30-40min in the retort furnace moving to and be warming up to 300 DEG C in advance after Homogeneous phase mixing into, crucible burned is in advance transferred in the retort furnace of 850-1000 DEG C and founds 30-40min.Finally, anneal glass metal 3h after copper coin top casting slivering at 300-450 DEG C, cools to room temperature with the furnace.Carry out test analysis after glass after annealing is polished into specific dimensions, result as shown in Figure 1 and Figure 2.The weight loss of glass sample in the synthetic perspiration of PH=4 is 8.33E-5mg/cm 2/ day, its T g, T fbe respectively 378 DEG C, 418 DEG C.

Claims (4)

1. be applied to a Unlead low-smelting point fluorphosphate glass for emerald filling, it is characterized in that the molar percentage of this glass consists of:
P 2O 5：20-40mol%，
B 2O 3：5-10mol%，
CaF 2:7-15mol%，
BaF 2:8-15mol%，
LiF:2-10mol%，
NaF:30-50mol%，
Said components and be 100mol%,
Wherein, P 2o 5can by primary ammonium phosphate (NH 4h 2pO 4) introduce, B 2o 3by boric acid (H 3bO 3) introduce.
2. be applied to the Unlead low-smelting point fluorphosphate glass of emerald filling as claimed in claim 1, it is characterized in that, this softening temperature being applied to the Unlead low-smelting point fluorphosphate glass of emerald filling is low to moderate 353 DEG C.
3. be applied to the Unlead low-smelting point fluorphosphate glass of emerald filling as claimed in claim 1, it is characterized in that, this chemical stability being applied to the Unlead low-smelting point fluorphosphate glass of emerald filling is excellent, without any physicochemical change in basic solution, in the acidic solution of PH=4, weight loss is lower than 4.53E-4mg/cm2/day.
4. be applied to a preparation method for the Unlead low-smelting point fluorphosphate glass of emerald filling as claimed in claim 1, it is characterized in that preparation method is as follows:
Take raw material by formula, after fully mixing, put into crucible; According to NH 4h 2pO 4for raw material, then crucible is put into the retort furnace pre-burning 30-40min being warming up to 300 DEG C; If use P 2o 5for raw material, then directly carry out the 3rd step; Crucible after pre-burning is transferred in the crucible of 850-1000 DEG C and is incubated 30-40min; Glass metal is shaped in copper coin top casting and is placed in the retort furnace that is warming up near second-order transition temperature the 3h that anneals, cool to room temperature with the furnace.
CN201610116144.2A 2016-03-02 2016-03-02 Glass material for filling emeralds and preparation method of glass material Pending CN105541110A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006182584A (en) * 2004-12-27 2006-07-13 Asahi Techno Glass Corp Filter glass for cutting near-infrared ray
JP2011251903A (en) * 2000-06-05 2011-12-15 Ohara Inc Optical glass suffering little change in refractive index by radiation of light
CN102653450A (en) * 2010-12-23 2012-09-05 肖特公开股份有限公司 Fluorophosphate glasses
JP5349721B2 (en) * 2000-06-05 2013-11-20 株式会社オハラ Optical glass with small refractive index change by light irradiation
CN103708727A (en) * 2012-09-29 2014-04-09 成都光明光电股份有限公司 Fluophosphate optical glass

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011251903A (en) * 2000-06-05 2011-12-15 Ohara Inc Optical glass suffering little change in refractive index by radiation of light
JP5349721B2 (en) * 2000-06-05 2013-11-20 株式会社オハラ Optical glass with small refractive index change by light irradiation
JP2006182584A (en) * 2004-12-27 2006-07-13 Asahi Techno Glass Corp Filter glass for cutting near-infrared ray
CN102653450A (en) * 2010-12-23 2012-09-05 肖特公开股份有限公司 Fluorophosphate glasses
CN103708727A (en) * 2012-09-29 2014-04-09 成都光明光电股份有限公司 Fluophosphate optical glass

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