CN102557469B - Method for preparing photon switching micro nanocrystalline-glass composite material by means of selective laser melting - Google Patents
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- CN102557469B CN102557469B CN201210049395.5A CN201210049395A CN102557469B CN 102557469 B CN102557469 B CN 102557469B CN 201210049395 A CN201210049395 A CN 201210049395A CN 102557469 B CN102557469 B CN 102557469B
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- 239000011521 glass Substances 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000002844 melting Methods 0.000 title claims abstract description 11
- 230000008018 melting Effects 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims description 40
- 239000002245 particle Substances 0.000 claims description 19
- 230000008859 change Effects 0.000 claims description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000008187 granular material Substances 0.000 claims description 14
- 230000005855 radiation Effects 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 10
- 241000931526 Acer campestre Species 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 239000005388 borosilicate glass Substances 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- -1 rare earth ytterbium ion Chemical class 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 4
- 230000004927 fusion Effects 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 3
- 239000005365 phosphate glass Substances 0.000 claims description 3
- 239000005368 silicate glass Substances 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000013307 optical fiber Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 18
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000087 laser glass Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005132 Calcium sulfide based phosphorescent agent Substances 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a method for preparing photon switching micro nanocrystalline-glass composite material by means of selective laser melting. Under laser irradiation, inorganic glass powder containing a selective laser absorption function material strongly absorbs laser melting, is quickly composited with the photon switching micro nanocrystalline, and is solidified in a cooling way to form the transparent photon switching micro nanocrystalline-glass composite material. The method is high in adaptability, can be used for carrying out composition selection and material preparation of the inorganic glass powder according to the operating wavelength of a laser device, and can be used for preparing different types of micro nanocrystalline-glass composite materials.
Description
Technical field:
The invention belongs to the optical function material field, relate in particular to a kind of selective laser melting and prepare the method that light is changed micro-nano crystalline substance-glass composite functional material.
Background technology:
The laser gain material adopts laser crystalline substance and rare earth laser glass mostly.The brilliant heat conductance of laser is good, it is high to gain, and is suitable for continuously and height repeats sharp penetrating, but can not meets the large-sized demand for development of laserable material, and simultaneously, also there are the weak points such as rare earth functional ionic doping is low, uniform doping is good not in the laser crystalline substance.The rare earth laser glass has that output rating is high, optical homogeneity good, price is lower, be easy to the advantages such as preparation, but the performances such as the thermal conductivity of material, laser generation threshold value, multiplicity are with the crystalline phase ratio, there is a big difference, easily introduce the impurity such as Pt, water in glass, and the problem such as easily split while having superpower, the material application is very limited.
Devitrified glass is the type material of a class between unorganic glass and crystalline substance, and it is crystallization highly, also can contain a large amount of glassy phases, very tempting for the laser field prospect.On the one hand, light emitting ionic can be implanted selectively crystallite mutually in, material is had and is similar to brilliant spectral signature, its inhomogeneous line width narrows down; On the other hand, material has the transparency and the thermostability of similar glass matrix, can carry out the large size preparation.But because devitrified glass exists that brilliant degree of crystallinity is not high, glass basis contains crystallization impurity and the weak point such as height crystallization situation lower-glass transparency is low, therefore, the devitrified glass prepared under the prior art condition also is difficult to meet laser glass superpower, high efficiency requirement.
With devitrified glass, compare, at the light of being changed micro-nano crystalline substance and unorganic glass matrix composition by light, change in micro-nano crystalline substance-glass composite functional material, the light of crystal property excellence is changed micro-nano crystalline substance and is played good light transformation, and unorganic glass matrix only plays the medium effect, do not introduce again rare earth ion and crystallization impurity simultaneously.Therefore, this micro-nano crystalline substance-glass composite functional material has overcome the limited and devitrified glass of single brilliant scantling and has easily introduced impurity, frangible shortcoming, again the distinct advantages of single crystalline substance and microcrystal glass material is organically united, be the very promising light transition function composite functional material of a class simultaneously.
In the micro-nano brilliant material of light conversion, the brilliant material of six rare earth ion doped side's phase fluorination things, as NaYbF
4, NaGdF
4, LiYbF
4, NaYF
4, LiYF
4deng, the material system phonon energy is low, is the best luminescent material system of finding up to now.But, the micro-nano brilliant material of light conversion of these excellent propertys is difficult to be incorporated in glass matrix by conventional method, major cause is that light changes in micro-nano crystalline substance-unorganic glass high-temperature fusion recombination process the micro-nano crystalline substance of conversion variation and the destruction by crystal formation easily occurs, and causes the luminescent properties of material significantly to descend.Adopt low melting glass matrix can reduce to a certain extent the combined heat treatment temperature that light is changed micro-nano crystalline substance-unorganic glass, but the thermotolerance of low melting glass matrix, acid-proof alkaline are difficult to meet service requirements.
Laser beam has the advantages such as energy density is high, radiation heating is fast, introduce specific laser absorption functional mass in the unorganic glass matrix of resistance to elevated temperatures excellence, can make unorganic glass matrix efficient absorption laser energy, realize that itself and light are changed the Flashmelt of micro-nano crystalline substance compound.The Flashmelt of unorganic glass matrix has reduced to greatest extent heat effect and light has been changed to the destruction of micro-nano crystalline substance, has guaranteed that light changes the light conversion properties energy of micro-nano crystalline substance-glass composite functional material integral body.At present, thisly utilize the selective laser melting to prepare high-performance optical to change the method for micro-nano crystalline substance-glass composite functional material and have not been reported.
Summary of the invention:
The objective of the invention is provides a kind of selective laser melting to prepare the method that light is changed micro-nano crystalline substance-glass composite functional material in order to improve existing light to change the deficiency of micro-nano crystalline substance-glass composite functional material and preparation method thereof.
Technical scheme of the present invention is: a kind of selective laser melting prepares the method that light is changed micro-nano crystalline substance-glass composite functional material, and its concrete steps are:
A) the scattered even shakedown of function composite granule is overlayed on to the glass in preheat mode or ceramic substrate surface in vacuum chamber, controlling function composite granule thickness is 5～100 μ m, wherein, the function composite granule is changed micro-nano crystalline substance and unorganic glass powder according to mass ratio (5～120) by light: 100 form;
B) by the inswept function composite granule of the laser beam homogeneous surface of laser apparatus emission, compound with the micro-nano brilliant rapid fusion of light conversion mixed after unorganic glass powder absorbing laser in the function composite granule, form transparent light and change micro-nano crystalline substance-glass laminated film after cooled and solidified;
C), according to thickness requirement repeating step A, B, obtain required light and change micro-nano crystalline substance-glass composite functional material.
Preferred steps A) thickness of controlling the function composite granule in is 10～30 μ m.The preheating temperature of substrate is 100～300 ℃.
Preferred described light is changed micro-nano crystalline substance and is at least any one in the micro-nano crystalline substance of conversion or the micro-nano crystalline substance of lower conversion, light change micro-nano crystalline substance to the laser of laser apparatus emission without a little less than absorbing or absorb extremely, and average particle size particle size is 30～800nm; Wherein, above change micro-nano crystalline substance into Yb
3+-Tm
3+the NaYF of co-doped
4, NaGdF
4or YAG, or Yb
3+-Er
3+the NaYF of co-doped
4, NaGdF
4or YAG, or Eu
3+-Sm
3+the CaS of co-doped or SrS, or Eu
3+-Dy
3+the CaS of co-doped or any one in SrS; Change micro-nano crystalline substance into Eu down
3+or Tb
3+the NaYF of doping
4, NaGdF
4or any one in YAG.
The particle size of preferred described unorganic glass powder is 0.5～20 μ m, preferably 1～10 μ m; The unorganic glass powder is any one in silicate glass, phosphate glass or the borosilicate glass that contains selective laser absorptive function material; In the unorganic glass powder, the mass percent of selective laser absorptive function material is 5～80%; Wherein, the functional mass of selectivity absorption 808nm wavelength laser is the rare earth dysprosium ion; The functional mass that selectivity absorbs the 980nm wavelength laser is the rare earth ytterbium ion; The functional mass that selectivity absorbs 1060nm, 1064nm wavelength laser is rare earth samarium ion or dysprosium ion; The functional mass that selectivity absorbs 10.6 mum wavelength laser is the oxide groups that contains silicon or phosphorus.
Any one in the laser that described laser apparatus is semiconductor light fibre laser, Nd:YAG laser apparatus or carbon dioxide laser radiation; The average power density of the laser beam of laser apparatus emission is 10
2～10
5w/cm
2; The sweep velocity of laser beam is 0.1～5 cel; Wherein, the optical maser wavelength of semiconductor optical fibre laser radiation be 808,980 or 1064nm in any one, the optical maser wavelength of Nd:YAG laser radiation is 1060nm or 1064nm, the optical maser wavelength of carbon dioxide laser radiation is 10.6 μ m.
Beneficial effect:
1, introduce specific selective laser absorptive function material in the high-performance glass component and can make glass material absorbing laser energy fast and efficiently, realize that glass matrix and light changes the rapid fusion of micro-nano crystalline substance.Crystalline structure and the performance that light is changed micro-nano crystalline substance both stablized in the use of this Flashmelt technology, guarantee that light changes micro-nano crystalline substance-glass composite functional material and have on the whole good chemical stability and resistance toheat.
The even shakedown of function composite granule that 2, will evenly mix overlays on the gasket surface of homogeneous heating, can function composite granule Flashmelt under lower laser beam power density.
3, the method strong adaptability, can carry out composition selection, design and the material preparation of unorganic glass powder according to the operation wavelength of laser apparatus, also be applicable to the preparation of the micro-nano crystalline substance of other types-glass composite functional material.
Embodiment:
Embodiment 1:
According to mass ratio 10: 100, the YAG:Eu that is 50nm by mean particle size
3+(1%) (silicate glass, the quality percentage composition is 72SiO to change the unorganic glass powder that micro-nano crystalline substance (commercially available) and mean particle size are 7.5 μ m under
2-3Al
2o
3-10Na
2o-10K
2o-5CaO, the oxide compound of Si is for absorbing the functional mass of 10.6 mum wavelength laser, its quality percentage composition is 72%, commercially available) make the complex function powder.Dispersed good complex function powder paving is overlayed on the quartz glass substrate that Heating temperature is 150 ℃, control thickness and be about at 22 μ m; Just (optical maser wavelength is 10.6 μ m to the laser of carbon dioxide laser radiation, and the laser beam power density is 2.2 * 10
4w/cm
2) inswept from the top layer of complex function powder with the speed of 5 cels, the complex function powder within 1 second Flashmelt, solidify and form transparent lower light and change micro-nano crystalline substance-glass laminated film; Repeat above step 5 time, obtain the micro-nano crystalline substance of lower conversion that thickness is about 90 μ m-glass composite film material.The nanocrystalline quality percentage composition of the thin-film material made is greater than 6%, and visible light transmissivity is greater than 80%, can by ultraviolet high efficiency be converted to the 610nm visible ray.
Embodiment 2:
According to mass ratio 40: 100, the β-NaYF that is 80nm by mean particle size
4: Yb
3+(20%), Tm
3+(2%) (borosilicate glass, the quality percentage composition is 60SiO to change the unorganic glass powder that micro-nano crystalline substance and mean particle size are 2.2 μ m on (commercially available)
2-20B
2o
3-10Na
2o-10CaO, the oxide compound of Si is for absorbing the functional mass of 10.6 mum wavelength laser, its quality percentage composition is 60%, commercially available) make the complex function powder.Dispersed good complex function powder paving is overlayed on the quartz glass substrate that Heating temperature is 280 ℃, control thickness and be about 13 μ m; By the laser of carbon dioxide laser radiation, (optical maser wavelength is 10.6 μ m, and the laser beam power density is 1.3 * 10
3w/cm
2) inswept from the top layer of complex function powder with the speed of 2 cels, the complex function powder within 2 seconds Flashmelt, solidify and form transparent light and change micro-nano crystalline substance-glass laminated film; Repeat above step 5 time, obtain the micro-nano crystalline substance of upper conversion that thickness is about 50 μ m-glass composite film material.In the micro-nano crystalline substance of the upper conversion made-glass composite functional material, nanocrystalline quality percentage composition is greater than 20%, and visible light transmissivity is greater than 80%, 0.98 μ m near infrared light can be converted to the 475nm visible ray efficiently.
Embodiment 3:
According to mass ratio 80: 100, the β-NaYF that is 500nm by mean particle size
4: Yb
3+(20%), Er
3+(2%) (rare-earth borosilicate glass, the quality percentage composition is 55SiO to change the unorganic glass powder that micro-nano crystalline substance and mean particle size are 1.1 μ m on (commercially available)
2-25B
2o
3-10Sm
2o
3-10BaO, Sm
3+for absorbing the functional mass of 1064nm wavelength laser, its corresponding oxide content is 10%, commercially available) make the complex function powder.Dispersed good complex function powder paving is overlayed on the quartz glass substrate that Heating temperature is 120 ℃, control thickness and be about 30 μ m; By the laser of Nd:YAG laser radiation, (optical maser wavelength is 1064nm, and the laser beam power density is 8.2 * 10
4w/cm
2) inswept from the top layer of complex function powder with the speed of 4.5 cels, the complex function powder within 1 second Flashmelt, solidify and form the transparent micro-nano crystalline substance of upper conversion-glass laminated film; Repeat above step 10 time, obtain the micro-nano crystalline substance of upper conversion that thickness is about 0.28mm-glass composite functional material.Micron crystalloid amount percentage composition of receiving in the film made is greater than 30%, and visible light transmissivity is greater than 70%, 0.98 μ m near infrared light can be converted to the 545nm visible ray efficiently.
Embodiment 4:
According to mass ratio 120: 100, the β-NaYF that is 300nm by mean particle size
4: Yb
3+(20%), Tm
3+(2%) (borosilicate glass, the quality percentage composition is 50SiO to change the unorganic glass powder that micro-nano crystalline substance and mean particle size are 4.4 μ m on (commercially available)
2-20B
2o
3-10Na
2o-10Yb
2o
3-10CaO, Yb
3+for absorbing the functional mass of 980nm wavelength laser, its corresponding oxide content is 10%, commercially available) make the complex function powder.Dispersed good complex function powder paving is overlayed on the quartz glass substrate that Heating temperature is 240 ℃, control thickness and be about 12 μ m; By the laser of semiconductor laser radiation, (wavelength is 980nm, and the laser beam power density is 2 * 10
2w/cm
2) inswept from the top layer of complex function powder with the speed of 0.5 cel, the complex function powder within 1 second Flashmelt, solidify and form the transparent micro-nano crystalline substance of upper conversion-glass composite functional material.In the film made, nanocrystalline quality percentage composition is greater than 40%, and visible light transmissivity is greater than 70%, 0.98 μ m near infrared light can be converted to the 475nm visible ray efficiently.
Embodiment 5:
According to mass ratio 5: 100, the CaS:Eu that is 25nm by mean particle size (0.015%), Dy (0.04%) above changes the unorganic glass powder that micro-nano crystalline substance (self-control) and mean particle size are 3.2 μ m, and (phosphate glass, the quality percentage composition is 50P
2o
5-20B
2o
3-10Al
2o
3-10Na
2o-10CaO, the oxide content of P is 50%) make the complex function powder.Dispersed good complex function powder paving is overlayed on the quartz glass substrate that Heating temperature is 150 ℃, control thickness and be about 16 μ m; By the laser of carbon dioxide laser radiation, (wavelength is 10.6 μ m, and the laser beam power density is 5 * 10
4w/cm
2) inswept from the top layer of complex function powder with the speed of 2 cels, the complex function powder within 1 second Flashmelt, solidify and form the transparent micro-nano crystalline substance of upper conversion-glass composite functional material.In the film made, nanocrystalline quality percentage composition is greater than 3%, and visible light transmissivity is greater than 70%, 0.98 μ m near infrared light can be converted to the 640nm visible ray efficiently.
Embodiment 6:
According to mass ratio 10: 100, the SrS:Eu that is 60nm by mean particle size (0.015%), Sm (0.04%) above changes the unorganic glass powder that micro-nano crystalline substance (self-control) and mean particle size are 2.8 μ m, and (borosilicate glass, the quality percentage composition is 50SiO
2-20B
2o
3-10Na
2o-15Dy
2o
3-5BaO, the oxide content of Dy is 15%) make the complex function powder.Dispersed good complex function powder paving is overlayed on the quartz glass substrate that Heating temperature is 200 ℃, control thickness and be about 30 μ m; By the semiconductor light fibre laser (select output wavelength 808nm, power 50W, the laser beam power density is 3 * 10
3w/cm
2) inswept from the top layer of complex function powder with the speed of 3 cels, the complex function powder within 1 second Flashmelt, solidify and form the transparent micro-nano crystalline substance of upper conversion-glass composite functional material.In the film made, nanocrystalline quality percentage composition is greater than 3%, and visible light transmissivity is greater than 70%, 0.98 μ m near infrared light can be converted to the 640nm visible ray efficiently.
Claims (6)
1. a selective laser melting prepares the method that light is changed micro-nano crystalline substance-glass composite functional material, and its concrete steps are:
A) the scattered even shakedown of function composite granule is overlayed on to the glass in preheat mode or ceramic substrate surface in vacuum chamber, controlling function composite granule thickness is 5～100 μ m; Wherein, the function composite granule is changed micro-nano crystalline substance and unorganic glass powder according to mass ratio (5～120) by light: 100 form; The preheating temperature of substrate is 100～300 ℃; The particle size of wherein said unorganic glass powder is 0.5～20 μ m; The unorganic glass powder is any one in silicate glass, phosphate glass or the borosilicate glass that contains selective laser absorptive function material; In the unorganic glass powder, the mass percent of selective laser absorptive function material is 5～80%; Wherein the functional mass of selectivity absorption 808nm wavelength laser is the rare earth dysprosium ion; The functional mass that selectivity absorbs the 980nm wavelength laser is the rare earth ytterbium ion; The functional mass that selectivity absorbs 1060nm, 1064nm wavelength laser is rare earth samarium ion or dysprosium ion; The functional mass that selectivity absorbs 10.6 mum wavelength laser is the oxide groups that contains silicon or phosphorus;
B) by the inswept function composite granule of the laser beam homogeneous surface of laser apparatus emission, compound with the micro-nano brilliant rapid fusion of light conversion mixed after unorganic glass powder absorbing laser in the function composite granule, form transparent light and change micro-nano crystalline substance-glass laminated film after cooled and solidified;
C), according to thickness requirement repeating step A, B, obtain required light and change micro-nano crystalline substance-glass composite functional material.
2. the method for claim 1, is characterized in that steps A) in function composite granule thickness be 10～30 μ m.
3. the method for claim 1, is characterized in that described light changes micro-nano crystalline substance and be at least any one in the micro-nano crystalline substance of conversion or the micro-nano crystalline substance of lower conversion; Average particle size particle size is 30～800nm.
4. method as claimed in claim 3, is characterized in that describedly above changing micro-nano crystalline substance into Yb
3+-Tm
3+the NaYF of co-doped
4, NaGdF
4or YAG, or Yb
3+-Er
3+the NaYF of co-doped
4, NaGdF
4or YAG, or Eu
3+-Sm
3+the CaS of co-doped or SrS, or Eu
3+-Dy
3+the CaS of co-doped or any one in SrS; Change micro-nano crystalline substance into Eu down
3+or Tb
3+the NaYF of doping
4, NaGdF
4or any one in YAG.
5. the method for claim 1, the particle size that it is characterized in that described unorganic glass powder is 1～10 μ m.
6. the method for claim 1, is characterized in that any one in laser that described laser apparatus is semiconductor light fibre laser, Nd:YAG laser apparatus or carbon dioxide laser radiation; The average power density of the laser beam of laser apparatus emission is 10
2～10
5w/cm
2; The sweep velocity of laser beam is 0.1～5 cel; Wherein, the optical maser wavelength of semiconductor optical fibre laser radiation be 808,980 or 1064nm in any one, the optical maser wavelength of Nd:YAG laser radiation is 1060nm or 1064nm, the optical maser wavelength of carbon dioxide laser radiation is 10.6 μ m.
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