CN102557440B - Preparation method for erbium-containing and neodymium-containing phosphorus germinate glass chip - Google Patents
Preparation method for erbium-containing and neodymium-containing phosphorus germinate glass chip Download PDFInfo
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- CN102557440B CN102557440B CN201210003058.2A CN201210003058A CN102557440B CN 102557440 B CN102557440 B CN 102557440B CN 201210003058 A CN201210003058 A CN 201210003058A CN 102557440 B CN102557440 B CN 102557440B
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Abstract
The invention relates to a preparation method for an erbium-containing and neodymium-containing phosphorus germinate glass chip. The method comprises the following steps: a, mixing 40 to 70 molar percent of phosphorus pentoxide, 0 to 7.5 molar percent of germanium dioxide, 4 to 20 molar percent of zinc oxide, 0 to 50 molar percent of zinc chloride, 0.5 to 1 molar percent of erbium oxide and 2 to 5 molar percent of neodymium oxide uniformly; b, placing a mixture into a covered quartz crucible or platinum crucible, placing into an electric furnace and melting at the temperature of 1,300 and 1,450 DEG C to form molten glass; c, homogenizing and clarifying the molten glass which is molten completely, discharging out of the furnace and quickly pouring in a preheated die; d, putting the formed glass into a muffle furnace which is heated to the glass transition temperature and annealing; and e, taking out the glass sample after the glass sample is cooled completely. The prepared phosphorus germinate glass has the characteristics of high transparency, strong crystallization resistance, excellent heat stability and physicochemical properties, stable near infrared laser property and the like.
Description
Technical field
The present invention relates to method for glass preparation, particularly relate to a kind of preparation method of the phosphorus bismuth germanate glass chip containing erbium, neodymium element of near-infrared laser output use.
Background technology
Near-infrared laser has broad application prospects at aspects such as laser medicine, eye-safe lidar, remote sensing, atmospheric surveillances, the particularly application aspect human body physical therapy, as treatment hyperlipidemia, reduction blood viscosity get more and more people's extensive concerning with prevention cardiovascular and cerebrovascular diseases, treatment cardiovascular and cerebrovascular disease and preventing hypertension etc.What generally adopt at present is that 650~780 nm visible red laser that semiconductor laser is sent directly act on human body.But the laser of this wave band because of wavelength bigger than normal compared with short energy.Energy is moderate near the infrared laser of wavelength 1 micron, is the desired wavelength of laser physical therapeutical instrument.A lot of substrate materials, as fused quartz, fluorochemical, germanate, phosphoric acid salt, doping neodymium in tellurate glass (Nd) ion all can obtain near-infrared laser and export (referring to John H. Campbell, Joseph S. Hayden, Alex Marker, High-Power Solid-State Lasers:a Laser Glass Perspective, International Journal of Applied Glass Science).Fluoride glass phonon energy very low (540 cm-1).But, because of features such as complicated process of preparation, chemical stability and the bad mechanical properties of above-mentioned substance, make its be difficult to practical industrialization (referring to J. Y Allain, M. Monerie, and H. Poignant, Room temperature cw tunable green upconversion holmium fiber laser, Electron. Lett. 1 990,26 (4): 261-262).Fused quartz glass has good physical properties, but its phonon energy higher (1100cm~1), and rare earth dissolving power is poor.Bismuth germanate glass also makes its application be restricted because of higher glass melting temperature and expensive raw materials cost.Comparatively speaking, phosphorus bismuth germanate glass has rational phonon energy, has better chemistry and mechanical stability and wider luminescent spectrum than phosphate glass.By mixing altogether with erbium (Er), can better reduce laser threshold, be easy to realize portable milliwatt level infrared laser output.
Summary of the invention
The present invention is intended to address the above problem, and provide, a kind of preparation technology is simple, cost is low, the phosphorus bismuth germanate glass transparency preparing is good, anti-crystallization ability is strong, thermostability and physical and chemical performance are good, the preparation method of the phosphorus bismuth germanate glass chip containing erbium, neodymium element of near-infrared laser stable performance.
For achieving the above object, the invention provides a kind of preparation method of the phosphorus bismuth germanate glass chip containing erbium, neodymium element, the method comprises the steps:
A, by the Vanadium Pentoxide in FLAKES of mole percent level 40~70, germanium dioxide 0~7.5, zinc oxide 4~20, zinc chloride 0~50, Erbium trioxide 0.5~1, Neodymium trioxide 2~5 mixes;
B, mixture is put into quartz pincers pot or the platinum pincers pot of adding a cover, and be placed in electric furnace, the temperature fusing of 1300~1450 DEG C, form glass melt;
C, will be completely come out of the stove after the glass melt homogenizing clarification that forms of fusing, be then cast in rapidly moulding on the mould of preheating;
D, the glass of moulding is put into the retort furnace that is warming up to glass transformation temperature anneal;
E, after completely cooling, take out glass sample.
Preferably, the method comprises the steps:
A, by the Vanadium Pentoxide in FLAKES of mole percent level 55, germanium dioxide 4, zinc oxide 12, zinc chloride 25, Erbium trioxide 0.7, Neodymium trioxide 3.3 mixes;
B, mixture is put into quartz pincers pot or the platinum pincers pot of adding a cover, and be placed in electric furnace, the temperature fusing of 1400 DEG C, form glass melt;
C, will be completely come out of the stove after the glass melt homogenizing clarification that forms of fusing, be then cast in rapidly moulding on the mould of preheating;
D, the glass of moulding is put into the retort furnace that is warming up to glass transformation temperature anneal;
E, after completely cooling, take out glass sample.
In step b, in the melting process of mixture, pass into drying nitrogen and carry out atmosphere protection.
In step c, the tapping temperature of the glass melt of fusing is 1000~1200 DEG C.
In steps d, described annealing process is glass transformation temperature insulation 2 hours, is then cooled to 100 DEG C with the speed of 2~5 DEG C/h, closes retort furnace power supply, is automatically cooled to room temperature.
Described glass transformation temperature is 436 DEG C~392 DEG C.
Contribution of the present invention is, the problem such as it efficiently solves prior art complicated process of preparation, chemical stability and bad mechanical property, preparation cost height.Because the present invention has added germanium dioxide and zinc oxide preparing in material, thereby formation ability and the mechanical property of glass system are effectively improved, improve the anti-crystallization ability of glass, make thermostability and the physical and chemical performance of glass good, reached practical requirement.Because the present invention has added zinc chloride (ZnCl2) preparing in material, and muriatic phonon energy is lower than fluorochemical, makes its phonon energy that has further reduced glass, thereby greatly reduces laser threshold.Also because the present invention has added erbium and neodymium element preparing in material, thereby effectively reduce laser threshold, thereby prepared glass is easy to as portable laser physiotherapy equipment chip.The present invention also has the features such as preparation technology is simple, cost is low, and the phosphorus bismuth germanate glass transparency preparing is good, and anti-crystallization ability is strong, and thermostability and physical and chemical performance are good, near-infrared laser stable performance.
Embodiment
The following example is further explanation of the present invention, and the present invention is not constituted any limitation.
Embodiment 1
Get 70 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 7.5 grams of germanium dioxides, 20 grams, zinc oxide, 0.5 gram of Erbium trioxide, 2 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1400 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1100 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast in to moulding on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 436 DEG C of material transition temperature (Tg) and anneals.In annealing process, first near 436 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, be then cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 590 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 436 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 154 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Embodiment 2
Get 60 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 7.5 grams of germanium dioxides, 10 grams, zinc oxide, 20 grams of zinc chloride, 0.5 gram of Erbium trioxide, 2 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1300 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1000 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 419 DEG C of material transition temperature (Tg) and anneals, in annealing process, first near 419 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, then be cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 582 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 419 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 163 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Embodiment 3
Get 50 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 4 grams of germanium dioxides, 10 grams, zinc oxide, 30 grams of zinc chloride, 1 gram of Erbium trioxide, 5 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1350 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1150 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 408 DEG C of material transition temperature (Tg) and anneals, in annealing process, first near 408 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, then be cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 543 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 408 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 135 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Embodiment 4
Get 45 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 5 grams of germanium dioxides, 7.5 grams, zinc oxide, 40 grams of zinc chloride, 0.5 gram of Erbium trioxide, 2 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1330 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1050 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 395 DEG C of material transition temperature (Tg) and anneals, in annealing process, first near 395 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, then be cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 534 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 395 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 139 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Embodiment 5
Get 45 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 4 grams of germanium dioxides, 5 grams, zinc oxide, 40 grams of zinc chloride, 1 gram of Erbium trioxide, 5 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1420 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1170 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 399 DEG C of material transition temperature (Tg) and anneals, in annealing process, first near 399 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, then be cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 550 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 399 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 151 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Embodiment 6
Get 40 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 7.5 grams, zinc oxide, 50 grams of zinc chloride, 0.5 gram of Erbium trioxide, 2 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1430 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1080 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 381 DEG C of material transition temperature (Tg) and anneals, in annealing process, first near 381 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, then be cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 523 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 381 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 142 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Embodiment 7
Get 40 grams of dusty raw materials Vanadium Pentoxide in FLAKESs, 5 grams of germanium dioxides, 4 grams, zinc oxide, 45 grams of zinc chloride, 1 gram of Erbium trioxide, 5 grams of Neodymium trioxide, mix above-mentioned raw materials.Mixture is put into quartz pincers pot or platinum pincers pot, on platinum pincers pot, add a cover to prevent Cl
-1volatilization.Be placed in globars electric furnace and found the quartz pincers pot of mixture or platinum pincers pot are housed, temperature of fusion is 1450 DEG C, founds in process, to pass into drying nitrogen and carry out atmosphere protection.Treat that raw material melts completely, and come out of the stove in 1200 DEG C after homogenizing clarification, after coming out of the stove, rapidly glass metal is cast on the swage tool of preheating.Then the glass of moulding being put into oneself is warming up near the retort furnace 392 DEG C of material transition temperature (Tg) and anneals, in annealing process, first near 392 DEG C of the transition temperatures (Tg) of this glass material, be incubated 2 hours, then be cooled to 100 DEG C with the speed of 3 DEG C/h, then close retort furnace power supply, be automatically cooled to room temperature.After completely cooling, take out glass sample, obtain the glass being made by glass composition of the present invention.
The differential thermal curve that the thermal stability of prepared glass records by differential thermal analyzer (DSC) is evaluated.The difference that the crystallization of glass starts temperature (Tx) and transition temperature (Tg) is larger, and anti-crystallization ability is stronger, shows that the thermostability of this glass is better.The glass of being prepared by the aforesaid method of the present embodiment after tested, it is 512 DEG C that its crystallization starts equilibrium temperature (Tx), its glass transformation temperature (Tg) is 392 DEG C, the fixed poor Tx-Tg of temperature that crystallization starts equilibrium temperature and transition temperature is 120 DEG C, the difference of this temperature is much larger than 100 DEG C, thereby there is good thermal stability energy, physical and chemical performance is good simultaneously, can meet the requirement of use completely, and the phosphorus bismuth germanate glass containing erbium, neodymium element being made by said process is transparent in crystallization, and physical and chemical performance is good.
Claims (3)
1. a preparation method for the phosphorus bismuth germanate glass chip containing erbium, neodymium element of exporting for near-infrared laser, is characterized in that, the method comprises the steps:
A, by the Vanadium Pentoxide in FLAKES of mole percent level 40~70, germanium dioxide 4~7.5, zinc oxide 4~20, zinc chloride 25~50, Erbium trioxide 0.5~1, Neodymium trioxide 2~5 mixes, the molar content sum of described each component is 100%;
B, mixture is put into quartz pincers pot or the platinum pincers pot of adding a cover, and be placed in electric furnace, the temperature fusing of 1300~1450 DEG C, form glass melt;
C, will be completely come out of the stove after the glass melt homogenizing clarification that forms of fusing, the tapping temperature of the glass melt of fusing is 1000~1200 DEG C, is then cast in rapidly moulding on the mould of preheating;
D, the glass of moulding is put into the retort furnace that is warming up to glass transformation temperature anneal, described annealing process is glass transformation temperature insulation 2 hours, then be cooled to 100 DEG C with the speed of 2~5 DEG C/h, close retort furnace power supply, automatically be cooled to room temperature, described glass transformation temperature is 436 DEG C~392 DEG C;
E, after completely cooling, take out glass sample.
2. the method for claim 1, is characterized in that, by the Vanadium Pentoxide in FLAKES of mole percent level 55, and germanium dioxide 4, zinc oxide 12, zinc chloride 25, Erbium trioxide 0.7, Neodymium trioxide 3.3 mixes;
B, mixture is put into quartz pincers pot or the platinum pincers pot of adding a cover, and be placed in electric furnace, the temperature fusing of 1400 DEG C, form glass melt;
C, will be completely come out of the stove after the glass melt homogenizing clarification that forms of fusing, be then cast in rapidly moulding on the mould of preheating;
D, the glass of moulding is put into the retort furnace that is warming up to glass transformation temperature anneal;
E, after completely cooling, take out glass sample.
3. the method for claim 1, is characterized in that, in step (b), passes into drying nitrogen and carry out atmosphere protection in the melting process of mixture.
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