CN108264217A - A kind of preparation process of neodymium doping laser quartz glass - Google Patents
A kind of preparation process of neodymium doping laser quartz glass Download PDFInfo
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- CN108264217A CN108264217A CN201810108290.XA CN201810108290A CN108264217A CN 108264217 A CN108264217 A CN 108264217A CN 201810108290 A CN201810108290 A CN 201810108290A CN 108264217 A CN108264217 A CN 108264217A
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- doping
- quartz
- neodymium
- quartz glass
- colloidal sol
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/235—Heating the glass
-
- 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
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
Abstract
The invention discloses a kind of preparation processes of neodymium doping laser quartz glass, sol method is combined with titration spray-on process, using six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent and water as raw material when prepared by colloidal sol, doping component is ranging from：Nd3+:0.5~1.2mol%, Al3+:0.4~6mol%, Ti4+：0~3mol%, Y3+:0~0.8mol%, surplus Si4+, shorter, Nd in the quartz pushrod of gained the time required to doping3+Ion doping can reach 2*10 at concentrations up to 0.8 3.5wt%, uniform doping‑4Magnitude；Quartz pushrod outer diameter can reach φ 30*150mm, Nd3+The peak emission section of ion>1.5x10~20cm2, melting technology advantage of lower cost, alternative existing Nd3+In terms of the phosphate glass and YAG crystal of doping are applied to laser impact intensified equipment and the power generation of the laser-produced fusion energy.
Description
Technical field
The present invention relates to the preparing technical field of quartz glass, specially a kind of system of neodymium doping laser quartz glass
Standby technique.The quartz glass prepared using this method can substitute existing Nd3+The phosphate glass of doping and YAG crystal applications
In terms of laser impact intensified equipment and the power generation of the laser-produced fusion energy.
Background technology
The laser material of 1 μm of section is directed to, whether xenon flash lamp pumping or LD are as pumping source, from reiforcing laser impact technology
For application with the power generation of the laser-produced fusion energy, laser material is required to Gao Zhongying thermal shock resistance, while its spectrum,
Laser activity is good enough.Proposed the laser material of a variety of possible applications both at home and abroad in recent years.Such as Yb-FAP, Nd/Yb-
YAG, Nd/Yb-CaF2, Nd/Yd-Glass etc..Wherein crystal (YAG) or transparent ceramic material generally have higher thermal conductivity
And higher emission cross section advantage, but the narrow unfavorable LD pumping matching of its absorption peak, while have that energy storage is poor, non-linear autohemagglutination
The shortcomings of burnt poor performance；And generally there is laser glass (N31) high-dopant concentration, high life energy storage, wide band absorption peak to be conducive to LD
The advantages that pumping source matching and large scale, but heat conductivility is excessively poor.Although Nd/Yb doping CaF2 crystal has also had many sharp
The advantages of light glass, but its existing fatal defects is that thermal expansion is too big, it is bigger than the existing N31 laser glasses coefficient of expansion
50%, therefore its heated caused deformation is larger.And the material damage threshold value of fluoride is relatively low, is easy to cause material heat
Distortion and generation fragmentation, larger impact is brought to the operation stability of whole system.
According to above analysis, although the poor thermal conductivity of laser glass material, but if it is made to have extremely low thermal expansion system
Number, then will be greatly reduced by thermally-induced laser glass impact failure, so as to improve the Gao Zhongying heat shock resistance of laser glass
Performance.The extremely low coefficient of thermal expansion of quartz glass meets this requirement well.Therefore it is most in terms of thermal shock resistance
Preferably, 12W/cm has been reached, has been 1.5 times of YAG.But Nd3+Nd in the quartz glass of doping3+Doping concentration relatively low lead
The defects of causing its spectrum low needs further to be promoted.
The patent of invention of Publication No. CN 106396378A discloses a kind of Nd3+The preparation side of Uniform Doped quartz glass
Method, Nd3+Uniform Doped is only up to 0.8moL%；The patent of invention of Publication No. CN 106495470A discloses neodymium ytterbium codope
Quartzy laser glass and preparation method thereof prepares porous silica loose powder using outside vapor deposition process and is placed in salt appearance
Doping is realized in easily, it is easy to adulterate uneven, lead to the impact resistance of material slightly to reduce；Publication No. CN 104016580B
The preparation method of the rear-earth-doped quartz glass bar of patent of invention use porous glass powder be impregnated in rare earth ion and codope
Leaching realized the doping of rare earth for 30~60 minutes in the mixed solution of ion, and the homogeneity of doping also is difficult to ensure.
Invention content
The technical problem to be solved by the present invention is to overcome existing Nd3+Nd in the quartz glass of doping3+Doping concentration compared with
Low the defects of causing its spectrum low, provides a kind of preparation process of neodymium doping laser quartz glass.
In order to solve the above technical problem, the present invention provides following technical solutions：
A kind of preparation process of neodymium doping laser quartz glass, includes the following steps：
One), the preparation of colloidal sol
With six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent
With water as raw material, doping component is ranging from：Nd3+:0.5~1.2mol%, Al3+:0.4~6mol%, Ti4+：0~
3mol%, Y3+:0~0.8mol%, surplus Si4+；Silicon alkoxide, water and organic solvent are sequentially added into six water after mixing
Neodymium chloride, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums are closed, stirs evenly and adjusts pH to proper range, preferably
PH is 7~8, is then placed in drum mixer, and stirring obtains colloidal sol after 2~5 hours；Preferably, silicon alkoxide：Water：It is organic
The mass ratio of solvent is：1:3.5~8:2~15；
Two), titration spraying
Colloidal sol is added in titration sprayer, colloidal sol is sprayed into the quartz round tube of spinning by the form of metered dose
Interior, quartz ampoule hull-skin temperature is heated to 1050 DEG C~1160 DEG C, and constant quartz ampoule internal temperature is 780 DEG C~820 DEG C, in height
Cl is passed through under temperature2Gas and oxygen purified and colloidal sol dehydration carbonization treatment, prepare Al-Ti-Nd-Y or Al-Ti-Nd,
Al-Nd-Y, Ti-Nd-Y are co-doped with quartz sand powder；Preferably, quartz ampoule hull-skin temperature is heated to 1100 DEG C, inside quartz ampoule
Constant temperature is 800 DEG C；
Three),
The doping silica flour of preparation is added in the graphite crucible of high frequency furnace, in the environment of helium is as protective gas
Be heated to 1500~1700 DEG C, silica flour made fully to melt the quartz glass liquid for bubble-free, by mouth of pot it is preset into
Type system releases solution, obtains the quartz pushrod of dimension after rapid cooling in air.
Further, it further includes and gained quartz pushrod is put into progress deshydroxy processing in the deshydroxy stove of vacuum degree 10-4pa.It is right
Size such as is sliced, is polished at the processing to deshydroxy treated quartz pushrod as required.
Sol method is combined by the preparation process of the neodymium doping laser quartz glass of the present invention with titration spray-on process, can
Good operability, it is shorter the time required to doping, have doping process, such as prepared using sol-gal process, required time about 3-5 days,
This method preparation time is only 6-8 hours, greatly shortens preparation time, improves working efficiency, it can be achieved that industrialization batch
The production of amount property；Nd in the quartz pushrod of gained3+Ion doping concentration is high, can reach 1.0-3.5wt%, uniform doping is good, reachable
To 2*10-4Magnitude；Quartz pushrod outer diameter can break through φ 20mm, reach φ 30*150mm, Nd3+The peak emission section of ion>
1.5x10~20cm2, melting technology advantage of lower cost, using coreless induction furnace as melting equipment, it can be achieved that industrial mass
Production, substitutes existing Nd3+The phosphate glass and YAG crystal of doping are applied to laser impact intensified equipment and laser-produced fusion energy
In terms of the power generation of source.
Specific embodiment
The preferred embodiment of the present invention is illustrated below, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
A kind of preparation process of neodymium doping laser quartz glass, includes the following steps：
One), the preparation of colloidal sol
With six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent
With water as raw material, doping component is ranging from：Nd3+:0.8mol%, Al3+:2mol%, Ti4+：1mol%, Y3+:
0.2mol%, surplus Si4+；It is according to mass ratio by silicon alkoxide, water and organic solvent：1:5:10 sequentially add after mixing
Six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums stir evenly and adjust pH to 7~8, then
It is put into drum mixer, stirring obtains colloidal sol after 2~5 hours；
Two), titration spraying
Colloidal sol is added in titration sprayer, colloidal sol is sprayed into the quartz round tube of spinning by the form of metered dose
Interior, quartz ampoule hull-skin temperature is heated to 1100 DEG C, and constant quartz ampoule internal temperature is 800 DEG C；It is passed through Cl at high temperature2Gas
It is purified with oxygen and colloidal sol is dehydrated carbonization treatment, prepared Al-Ti-Nd-Y, Al-Ti-Nd and Ti-Nd-Y and be co-doped with quartz
Emery dust body；
Three),
The doping silica flour of preparation is added in the graphite crucible of high frequency furnace, in the environment of helium is as protective gas
1600 DEG C are heated to, silica flour is made fully to melt the quartz glass liquid for bubble-free, passes through the preset formation system of mouth of pot
Solution is released, obtains the quartz pushrod of dimension after rapid cooling in air.Gained quartz pushrod is put into vacuum degree 10-
Deshydroxy processing is carried out in the deshydroxy stove of 4pa, size is sliced, the processing such as polishes as required to deshydroxy treated quartz pushrod.
Embodiment 2
A kind of preparation process of neodymium doping laser quartz glass, includes the following steps：
One), the preparation of colloidal sol
With six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent
With water as raw material, doping component is ranging from：Nd3+:1.2mol%, Al3+:6mol%, Ti4+：3mol%, surplus Si4+；
According to silicon alkoxide：Water：The mass ratio of organic solvent is：1:3.5:15；By silicon alkoxide, water and organic solvent after mixing successively
Six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums are added in, stirs evenly and adjusts pH to 7~8,
It is then placed in drum mixer, stirring obtains colloidal sol after 2~5 hours；
Two), titration spraying
Colloidal sol is added in titration sprayer, colloidal sol is sprayed into the quartz round tube of spinning by the form of metered dose
Interior, quartz ampoule hull-skin temperature is heated to 1050 DEG C, and constant quartz ampoule internal temperature is 780 DEG C, is passed through Cl at high temperature2Gas
It is purified with oxygen and colloidal sol is dehydrated carbonization treatment, prepare Al-Ti-Nd quartz sand powders；
Three),
The doping silica flour of preparation is added in the graphite crucible of high frequency furnace, in the environment of helium is as protective gas
1500 DEG C are heated to, silica flour is made fully to melt the quartz glass liquid for bubble-free, passes through the preset formation system of mouth of pot
Solution is released, obtains the quartz pushrod of dimension after rapid cooling in air.
Embodiment 3
A kind of preparation process of neodymium doping laser quartz glass, includes the following steps：
One), the preparation of colloidal sol
With six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent
With water as raw material, doping component is ranging from：Nd3+:0.5mol%, Al3+:0.4mol%, Y3+:0.8mol%, surplus are
Si4+；By silicon alkoxide, water and organic solvent according to mass ratio be 1:8:2 sequentially add six Neodymium chloride hydrates, six water after mixing
Aluminium chloride, nano-titanium dioxide, six chloride hydrate yttriums are closed, stirs evenly and adjusts pH to 7~8, be then placed in drum mixer
Interior, stirring obtains colloidal sol after 2~5 hours；
Two), titration spraying
Colloidal sol is added in titration sprayer, colloidal sol is sprayed into the quartz round tube of spinning by the form of metered dose
Interior, quartz ampoule hull-skin temperature is heated to 1160 DEG C, and constant quartz ampoule internal temperature is 820 DEG C, is passed through Cl at high temperature2Gas
It is purified with oxygen and colloidal sol is dehydrated carbonization treatment, prepare Al-Nd-Y quartz sand powders；
Three),
The doping silica flour of preparation is added in the graphite crucible of high frequency furnace, in the environment of helium is as protective gas
1700 DEG C are heated to, silica flour is made fully to melt the quartz glass liquid for bubble-free, passes through the preset formation system of mouth of pot
Solution is released, obtains the quartz pushrod of dimension after rapid cooling in air.Gained quartz pushrod is put into vacuum degree 10-
Deshydroxy processing is carried out in the deshydroxy stove of 4pa.
Embodiment 4
A kind of preparation process of neodymium doping laser quartz glass, includes the following steps：
One), the preparation of colloidal sol
With six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent
With water as raw material, doping component is ranging from：Nd3+:1.0mol%, Al3+:4mol%, Ti4+：2mol%, Y3+:
0.6mol%, surplus Si4+；It is according to mass ratio by silicon alkoxide, water and organic solvent：1:6:12 sequentially add after mixing
Six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums stir evenly and adjust pH to 7~8, then
It is put into drum mixer, stirring obtains colloidal sol after 2~5 hours；
Two), titration spraying
Colloidal sol is added in titration sprayer, colloidal sol is sprayed into the quartz round tube of spinning by the form of metered dose
Interior, quartz ampoule hull-skin temperature is heated to 1100 DEG C, and constant quartz ampoule internal temperature is 800 DEG C, is passed through Cl at high temperature2Gas
It is purified with oxygen and colloidal sol is dehydrated carbonization treatment, prepared Al-Ti-Nd-Y and Al-Nd-Y, Ti-Nd-Y are co-doped with quartz sand
Powder；
Three),
The doping silica flour of preparation is added in the graphite crucible of high frequency furnace, in the environment of helium is as protective gas
1650 DEG C are heated to, silica flour is made fully to melt the quartz glass liquid for bubble-free, passes through the preset formation system of mouth of pot
Solution is released, obtains the quartz pushrod of dimension after rapid cooling in air；Gained quartz pushrod is put into vacuum degree 10-4pa
Deshydroxy stove in carry out deshydroxy processing.To deshydroxy treated quartz pushrod, size is sliced, the processing such as polishes as required.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (5)
1. a kind of preparation process of neodymium doping laser quartz glass, which is characterized in that include the following steps：
One), the preparation of colloidal sol
With six Neodymium chloride hydrates, Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums, silicon alkoxide, organic solvent and water
As raw material, doping component is ranging from：Nd3+:0.5~1.2mol%, Al3+:0.4~6mol%, Ti4+：0~3mol%, Y3 +:0~0.8mol%, surplus Si4+；By silicon alkoxide, water and organic solvent sequentially add after mixing six Neodymium chloride hydrates,
Aluminium chloride hexahydrate, nano-titanium dioxide, six chloride hydrate yttriums stir evenly and adjust pH to proper range, are then placed in roller
In formula blender, stirring obtains colloidal sol after 2~5 hours；
Two), titration spraying
Colloidal sol is added in titration sprayer, is sprayed into colloidal sol in the quartz round tube of spinning by the form of metered dose, stone
English tube outer surface temperature is heated to 1050 DEG C~1160 DEG C, and constant quartz ampoule internal temperature is 780 DEG C~820 DEG C, at high temperature
It is passed through Cl2Gas and oxygen is purified and colloidal sol dehydration carbonization treatment, prepares Al-Ti-Nd-Y or Al-Ti-Nd, Al-Nd-
Y, Ti-Nd-Y is co-doped with quartz sand powder；
Three), prepared by neodymium doping quartz pushrod
The doping silica flour of preparation is added in the graphite crucible of high frequency furnace, is heated in the environment of helium is as protective gas
To 1500~1700 DEG C, silica flour is made fully to melt the quartz glass liquid for bubble-free, pass through the preset molding system of mouth of pot
System releases solution, obtains the quartz pushrod of dimension after rapid cooling in air.
2. the preparation process of neodymium doping laser quartz glass as described in claim 1, which is characterized in that the step
One) silicon alkoxide in：Water：The mass ratio of organic solvent is：1:3.5~8:2~15.
3. the preparation process of neodymium doping laser quartz glass as described in claim 1, which is characterized in that the step
Two) quartz ampoule hull-skin temperature is heated to 1100 DEG C in, and constant quartz ampoule internal temperature is 800 DEG C.
4. the preparation process of neodymium doping laser quartz glass as described in claim 1, which is characterized in that further include institute
It obtains quartz pushrod and is put into progress deshydroxy processing in the deshydroxy stove of vacuum degree 10-4pa.
5. the preparation process of neodymium doping laser quartz glass as described in claim 1, which is characterized in that further include to de-
Hydroxyl treated quartz pushrod as required size be sliced, polishing treatment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713343A (en) * | 2019-11-07 | 2020-01-21 | 南京工业大学东海先进硅基材料研究院 | Method for preparing doped quartz sand by cerium-aluminum co-doping |
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| CN1583620A (en) * | 2004-06-01 | 2005-02-23 | 中国科学院上海光学精密机械研究所 | Production of Nd doped high silicon-oxygen laser glass |
| CN101554491A (en) * | 2009-05-27 | 2009-10-14 | 四川大学 | Method for preparing bioactive glass coating by liquid-phase thermal spray |
| DE102013015934A1 (en) * | 2013-09-18 | 2015-03-19 | Friedrich-Schiller-Universität Jena | Rare earth doped aluminosilicate glasses, especially for use as active lasant material in high performance bulk lasers |
| CN106242277A (en) * | 2016-08-04 | 2016-12-21 | 江苏圣达石英制品有限公司 | A kind of rear-earth-doped water process quartz ampoule and preparation method thereof |
| CN106396378A (en) * | 2016-09-08 | 2017-02-15 | 中国科学院上海光学精密机械研究所 | Preparation method of Nd3+ uniformly doped quartz glass |
| CN107619185A (en) * | 2017-09-30 | 2018-01-23 | 徐传龙 | A kind of continuous induction melting furnace draws neodymium element laser quartz pushrod and preparation method thereof |
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2018
- 2018-02-02 CN CN201810108290.XA patent/CN108264217A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1583620A (en) * | 2004-06-01 | 2005-02-23 | 中国科学院上海光学精密机械研究所 | Production of Nd doped high silicon-oxygen laser glass |
| CN101554491A (en) * | 2009-05-27 | 2009-10-14 | 四川大学 | Method for preparing bioactive glass coating by liquid-phase thermal spray |
| DE102013015934A1 (en) * | 2013-09-18 | 2015-03-19 | Friedrich-Schiller-Universität Jena | Rare earth doped aluminosilicate glasses, especially for use as active lasant material in high performance bulk lasers |
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| CN110713343A (en) * | 2019-11-07 | 2020-01-21 | 南京工业大学东海先进硅基材料研究院 | Method for preparing doped quartz sand by cerium-aluminum co-doping |
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