CN104577699A - Diffusion bonding method of recombination laser media - Google Patents
Diffusion bonding method of recombination laser media Download PDFInfo
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- CN104577699A CN104577699A CN201410849950.1A CN201410849950A CN104577699A CN 104577699 A CN104577699 A CN 104577699A CN 201410849950 A CN201410849950 A CN 201410849950A CN 104577699 A CN104577699 A CN 104577699A
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Abstract
The invention provides a diffusion bonding method of recombination laser media, and aims at providing a method which is high in controllability and good in performance. The diffusion bonding method is achieved according to the following technical scheme: two or more media are selected from ceramic or crystals firstly; optical machining is carried out on the selected media; the two or more media are washed through ethyl alcohol to be placed into 10%-20% mixed acid with a ratio of sulfuric acid to phosphoric acid being 1:5; the media are taken out from the acid liquor to be washed, and then bonding faces are coated with silica gel for gluing and pressed through a molybdenum clamp; a pressed composite body of the ceramic or the crystals is placed into a muffle furnace to be slowly heated to 300 DEG C, heat preservation is carried out for three to ten hours, then the temperature slowly rises to 800 DEG C for heat preservation, and then the temperature slowly drops to the indoor temperature. Then the composite body is taken out from the muffle furnace to be placed into a vacuum sintering furnace, heat preservation is carried at the temperature ranging from 1600 DEG C to 1800 DEG, and finally the temperature slowly drops to the indoor temperature. The prepared recombination media are placed into an atmosphere sintering furnace, heat preservation at the temperature ranging from 1200 DEG C to 1500 DEG in the hydrogen or oxygen or air atmosphere is carried out for 40 hours to 200 hours, and then the temperature slowly drops to the indoor temperature.
Description
Technical field
The present invention relates to optical field, specifically the present invention relates to a kind of preparation method of diffusion interlinked composite laser medium.
Background technology
Laser medium is the core component of solid statelaser.Laser working medium is generally the single entirety of same monocrystalline, pottery or glass, as Nd:YAG crystal bar, Nd:YAG crystal microchip, Nd:YAG crystal lath, neodymium glass etc.In the solid statelaser of pulse or non-stop run, the heat that the radiation of laser medium absorptive pumping produces constitutes to the cooling of medium the thermal gradient that media interior has with outside, cause the various heat effect in medium, such as thermic stress birefringence, due to pumping section thermal stresses excessive and cause the breaking of crystal, thermal lensing effect etc.Along with the development of high power solid state laser, the heat management problems of this single operation material is more outstanding, limits laser power and beam quality.Heat effect has become obstruction and has obtained one of key factor of more high-output power and better beam quality.
In order to effectively control the heat effect problem of laser medium, the composite laser medium that people start to explore utility excellence replaces single laser medium.When physical condition is identical, composite laser medium more effectively suppresses heat effect problem than single laser medium, and beam quality and power also improve significantly.In the bonding techniques of the laser crystalss such as Nd:YAG, Yb:YAG, GGG, YLF that the U.S., Japan, Britain, Russia etc. grasp, the people such as Bagayev publish thesis on " OpticalMaterials " " Simple method to join YAG ceramics and crystals " (see Opt.Mater., 2012 (34): 951-954) discloses a kind of preparation method preparing the complex media of YAG pottery and crystal.First sintering prepares Nd:YAG pottery, then to the polishing of ceramic Nd:YAG and YAG monocrystalline, then plates one deck SiOx film and optical cement compression by magnetron sputtering at bonding surface, eventually pass and obtain complex media higher than 1700 DEG C of thermal treatments.But the method that the people such as Bagayev adopts is too complicated, poor controllability, do not consider yet pottery and crystal homogeneity or heterogeneous diffusion interlinked before chemical activation process is carried out to it.
Summary of the invention
The object of the invention is the weak point existed for above-mentioned prior art, provide a kind of simple to operate, controllability is strong, and the diffusion interlinked method of composite laser medium of good performance, to solve the problem of prior art heat effect difference.
The present invention have devised novel working-laser material, this working-laser material is no longer single operation material, but by multiple (comprising one) single laser ceramics and other pottery or crystal through diffusion interlinked technique, the operation material be bonded together, is called recombination laser working medium.
Above-mentioned purpose of the present invention can be reached by following measures, and a kind of diffusion interlinked method of composite laser medium, is characterized in that comprising the steps:
A diffusion interlinked method for composite laser medium, is characterized in that comprising the steps:
(1) selection and light add: rare-earth-dopping yttrium aluminum garnet (Re
xy
3-xal
5o
12) laser ceramics, rare earth doped yttrium oxide (Re
xy
2-xo
3) laser ceramics, rear-earth-doped oxidation scandium (Re
xsc
2-xo
3) laser ceramics, rear-earth-doped oxidation lutetium (Re
xlu
2-xo
3) laser ceramics, yttrium aluminum garnet (YAG) pottery, yttrium oxide (Y
2o
3) ceramic, Scium trioxide (Sc
2o
3) ceramic, lutecium oxide (Lu
2o
3) pottery, yttrium aluminum garnet (YAG) crystal, yttrium oxide (Y
2o
3) crystal, Scium trioxide (Sc
2o
3) crystal, lutecium oxide (Lu
2o
3) crystal, sapphire (Al
2o
3), from above-mentioned pottery or crystal, choose two pieces or polylith; Optical manufacturing is carried out again to choosing medium.
(2) chemical activation and gluing: by the above-mentioned optics three grades of media that reach after alcohol washes, put into 10% ~ 20%, sulfuric acid volume: phosphoric acid volume=1:5 mixing acid in pickling 10 ~ 40 minutes; Take out peace and quiet, exert pressure with the fixing complex body of molybdenum fixture machinery, add silica gel promote atomic diffusion at medium bonding surface, gluing is complex body;
(3) thermal pretreatment: the pottery make gluing clamping pressure or the complex media of crystal are put into muffle furnace and be slowly warmed up to 300 DEG C of insulations 3 ~ 10 hours, is slowly warmed up to 800 DEG C of insulations 20 ~ 60 hours, is then slowly down to room temperature.
(4) vacuum high-temperature thermal treatment: complex body is put into vacuum sintering furnace, in vacuum tightness 10
-3~ 10
-5pa, 1600 ~ 1800 DEG C insulation 10 ~ 30 hours, be slowly down to room temperature subsequently.
(5) anneal: the complex media obtained is put into atmosphere sintering furnace, under hydrogen, oxygen or air atmosphere, 1200 ~ 1500 DEG C are incubated 40 ~ 200 hours, are down to room temperature subsequently.
The present invention has following beneficial effect compared to existing technology
Present invention employs doped garnet laser ceramics, oxide compound laser ceramics and do not mix monocrystalline, ceramic bonding, applying a small amount of silica gel by simple method in the conjunction face that medium is tied carries out gluing, silica gel is utilized to promote diffusion interlinked, prepared composite laser medium is functional, can effectively improve superpower laser thermal characteristics and beam quality.
The present invention before diffusion interlinked, to utilizing the mixing acid of 10% ~ 20% (sulfuric acid volume: phosphoric acid volume=1:5) to carry out chemical activation process to pottery or plane of crystal, facilitate the diffusion of atom between bonding face, enhancing bond strength.
The present invention in the process of diffusion interlinked complex media, now doping laser ceramics with do not mix monocrystalline, polishing is carried out in ceramic bond contact face successively, chemical activation, gluing, add the controllability of bonding combined laser medium.
The present invention is at 1600 DEG C ~ 1800 DEG C, 20 kilograms/cm
2~ 40 kilograms/cm
2condition under make SiO
xcan impel in high temperature, high-pressure process doped ceramics with do not mix monocrystalline, pottery form bonding.
Complex media of the present invention is annealed in a hydrogen atmosphere and effectively can be eliminated the Minute pores of compound bonded interface.The present invention can provide compound (pottery or crystal) laser medium.
Accompanying drawing explanation
The diffusion bond process flow sheet of Fig. 1 composite laser medium of the present invention.
The composite laser medium C1/S schematic diagram that Fig. 2 the present invention is diffusion interlinked.
The composite laser medium C1/C schematic diagram that Fig. 3 the present invention is diffusion interlinked.
Fig. 4 diffusion interlinked composite laser medium S/C1/S schematic diagram of the present invention.
Fig. 5 diffusion interlinked composite laser medium C1/C2/S schematic diagram of the present invention.
Embodiment
Be described further below by the bonding method of embodiment to composite laser medium of the present invention.
Consult Fig. 1.According to the present invention, the diffusion interlinked concrete steps of composite laser medium comprise:
(1) selection: two pieces that choose or polylith medium, Re
xy
3-xal
5o
12, Re
xy
2-xo
3, Re
xsc
2-xo
3, Re
xlu
2- xo
3wherein X is 0.01 ~ 0.6, Re is neodymium (Nd), at least one in erbium (Er), cerium (Ce), holmium (Ho), thulium (Tm), europium (Eu) and chromium (Cr) mixes laser ceramics, and YAG, Y
2o
3, Sc
2o
3, Lu
2o
3, Al
2o
3at least one crystal do not mixed or the pottery do not mixed; Two pieces or polylith medium are same media, or not same media.
(2) light adds: the smooth finish in conjunction with plane of above-mentioned two pieces or polylith medium is reached optics three grades, planeness λ/4, f number N=0.5.
(3) chemical activation: by the above-mentioned optics three grades of media that reach after alcohol washes, put into 10% ~ 20%, sulfuric acid volume: phosphoric acid volume=1:5 mixing acid in pickling 10 ~ 40 minutes;
(4) gluing: medium is taken out from above-mentioned acid solution, with alcohol washes, then carry out gluing at the silica gel that the bonding surface of medium applies 0.2 milliliter ~ 0.8 milliliter, and use molybdenum fixture 20 kilograms/cm
2~ 40 kilograms/cm
2pressure compresses;
(5) thermal pretreatment: the pottery make gluing clamping pressure or the complex media of crystal are put into muffle furnace and be slowly warmed up to 300 DEG C of insulations 3 ~ 10 hours, is slowly warmed up to 800 DEG C of insulations 20 ~ 60 hours, is then slowly down to room temperature.
(6) vacuum high-temperature thermal treatment: complex body is put into vacuum sintering furnace, in vacuum tightness 10
-3~ 10
-5pa, 1600 ~ 1800 DEG C insulation 10 ~ 30 hours, be slowly down to room temperature subsequently.
(7) anneal: the complex media prepared is put into atmosphere sintering furnace, under hydrogen, oxygen or air atmosphere, 1200 ~ 1500 DEG C are incubated 40 ~ 200 hours, are down to room temperature subsequently.
The diffusion of diffusion interlinked dependence complex media bonding surface surface atom.Atomic diffusion mainly comprises: the movement three kinds closing on the exchange of atom, the movement of interstitial atom and hole.General requirement Heating temperature be they separately fusing point about 80%, bonding medium must be as far as possible close, and mating surface must be smooth and smooth.Adding in thermal diffusion process, using fixture machinery mounting medium and exert pressure and add silica gel promotion atomic diffusion at bonding surface.
Embodiment 1
By diameter 10 millimeters, the Nd of high 1 millimeter
0.06: Y
2.94al
5o
12ceramic disks and diameter 10 millimeters, high 5 millimeters of Y
3al
5o
12crystal wafers carries out light and adds, and requires that the smooth finish of bonding surface is at optics three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 10 minutes of 10% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.2 milliliter, silica gel, carries out gluing, and compress (20 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 3 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 20 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Nd
0.06y
2.94al
5o
12pottery is put into vacuum sintering furnace with the complex body of monocrystalline and is sintered, and vacuum tightness is 1 × 10
-3pa, by sintering procedure, 10 DEG C/min are manually warming up to 600 DEG C, then change time variable control, the temperature rise period: 600 ~ 1600 DEG C, and heat-up rate is 10 DEG C/min; Holding stage: 1600 DEG C are incubated 10 hours; Temperature-fall period: 1600 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Nd
0.06y
2.94al
5o
12pottery puts into oxygen atmosphere stove anneal with the complex media of monocrystalline.Program is as follows.Temperature rise period: room temperature ~ 1200 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 1200 DEG C are incubated 40 hours; Temperature-fall period: 1200 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 2
By long 40 millimeters, wide 20 millimeters, high 1.5 millimeters Ce
0.03: Y
2.97al
5o
12pottery lath and long 40 millimeters, wide 20 millimeters, high 5 millimeters of Y
3al
5o
12pottery lath carries out light and adds, and requires that the smooth finish of bonding surface is at optics more than three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 40 minutes of 20% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.8 milliliter, silica gel, carries out gluing, and compress (40 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 10 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 60 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Ce
0.03: Y
2.97al
5o
12ceramic Composite medium is put into vacuum sintering furnace and is sintered, and vacuum tightness is 1 × 10
-5pa, sintering procedure is as follows.Manually be warming up to 600 DEG C with 10 DEG C/min, then change time variable control, the temperature rise period: 600 ~ 1750 DEG C, heat-up rate is 10 DEG C/min; Holding stage: 1750 DEG C are incubated 30 hours; Temperature-fall period: 1750 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Ce
0.03: Y
2.97al
5o
12ceramic Composite medium puts into hydrogen atmosphere stove anneal, and program is as follows.Temperature rise period: room temperature ~ 1500 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1500 DEG C are incubated 200 hours; Temperature-fall period: 1400 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 3
By diameter 20 millimeters, high 2 millimeters of Y
3al
5o
12crystal wafers, diameter 20 millimeters, high 2 mm H o
0.6: Y
2.4al
5o
12pottery, diameter 20 millimeters, high 5 millimeters of Y
3al
5o
12crystal wafers carries out light and adds, and requires that the smooth finish of bonding surface is at optics more than three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 40 minutes of 20% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.5 milliliter, silica gel, carries out gluing, and compress (40 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 10 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 60 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Ho
0.6: Y
2.4al
5o
122ceramic Composite medium is put into vacuum sintering furnace and is sintered, and vacuum tightness is 5 × 10
-5pa, sintering procedure is as follows, is manually warming up to 600 DEG C, then changes time variable control, the temperature rise period with 10 DEG C/min: 600 ~ 1720 DEG C, and heat-up rate is 10 DEG C/min; Holding stage: 1720 DEG C are incubated 30 hours; Temperature-fall period: 1750 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Ho
0.6: Y
2.4al
5o
12ceramic Composite medium puts into hydrogen atmosphere stove anneal, and program is as follows.Temperature rise period: 0 ~ 1500 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1500 DEG C are incubated 200 hours; Temperature-fall period: 1400 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 4
By the length of side 15 millimeters, high 1 millimeter of Yb
0.015: Y
2.985al
5o
12pottery square, 15 millimeters, high 1.5 millimeters of Yb
0.6: Y
2.4al
5o
12pottery square and 15 millimeters, high 5 millimeters of Y
3al
5o
12crystal square carries out light and adds, and requires that the smooth finish of bonding surface is at optics three grades, planeness λ/4, f number N=0.5.By three pieces of media after alcohol washes, put into the mixing acid 30 minutes of 15% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.4 milliliter, silica gel, carries out gluing, and compress (30 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 8 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 20 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Yb
0.015: Y
2.985al
5o
12pottery, Yb
0.6: Y
2.4al
5o
12sinter in pottery and the complex body vacuum sintering furnace of monocrystalline, vacuum tightness is 1 × 10
-5pa, sintering procedure is as follows.Manually be warming up to 600 DEG C with 10 DEG C/min, then change time variable control, the temperature rise period: 600 ~ 1750 DEG C, heat-up rate is 10 DEG C/min; Holding stage: 1750 DEG C are incubated 20 hours; Temperature-fall period: 1750 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally pottery and the complex body of monocrystalline are put into hydrogen atmosphere stove anneal, program is as follows.Temperature rise period: room temperature ~ 1400 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1400 DEG C are incubated 150 hours; Temperature-fall period: 1400 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 5
By diameter 10 millimeters, high 1 millimeter of Er
0.01: Y
1.99o
3pottery and diameter 10 millimeters, high 6 millimeters of Y
2o
3crystal carries out light and adds, and requires that the smooth finish of bonding surface is at optics three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 20 minutes of 20% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.3 milliliter, silica gel, carries out gluing, and compress (20 kilograms/cm
2~ 40 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 10 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 30 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Er
0.01: Y
1.99o
3pottery is put into vacuum sintering furnace with the complex body of monocrystalline and is sintered, and vacuum tightness is 1 × 10
- 5pa, sintering procedure is as follows.Manually be warming up to 600 DEG C with 10 DEG C/min, then change time variable control, the temperature rise period: 600 ~ 1800 DEG C, heat-up rate is 10 DEG C/min; Holding stage: 1800 DEG C are incubated 15 hours; Temperature-fall period: 1800 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Er
0.01: Y
1.99o
3pottery puts into hydrogen atmosphere stove anneal with the complex body of monocrystalline, and program is as follows.Temperature rise period: room temperature ~ 1450 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1450 DEG C are incubated 200 hours; Temperature-fall period: 1450 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 6
By diameter 15 millimeters, high 2 millimeters of Cr
0.01: Sc
1.99o
3pottery and diameter 15 millimeters, high 4 millimeters of Sc
2o
3crystal carries out light and adds, and requires that the smooth finish of bonding surface is at optics three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 30 minutes of 20% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.4 milliliter, silica gel, carries out gluing, and compress (20 kilograms/cm
2~ 40 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 7 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 30 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Cr
0.01: Sc
1.99o
3pottery is put into vacuum sintering furnace with the complex body of monocrystalline and is sintered, and vacuum tightness is 5 × 10
- 5pa, sintering procedure is as follows.Manually be warming up to 600 DEG C with 10 DEG C/min, then change time variable control, the temperature rise period: 600 ~ 1780 DEG C, heat-up rate is 10 DEG C/min; Holding stage: 1780 DEG C are incubated 20 hours; Temperature-fall period: 1780 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Cr
0.01: Sc
1.99o
3pottery puts into hydrogen atmosphere stove anneal with the complex body of monocrystalline, and program is as follows.Temperature rise period: room temperature ~ 1400 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1400 DEG C are incubated 200 hours; Temperature-fall period: 1400 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 7
By the diameter 25 millimeters of purchase, the Tm of high 2 millimeters
0.03y
2.97al
5o
12pottery and diameter 25 millimeters, high 5 millimeters of Al
2o
3crystal carries out light and adds, and requires that the smooth finish of bonding surface is at optics three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 40 minutes of 15% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.5 milliliter, silica gel, carries out gluing, and compress (40 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 10 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 30 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Tm
0.03y
2.97al
5o
12pottery is put into vacuum sintering furnace with the complex body of monocrystalline and is sintered, and vacuum tightness is 1 × 10
-5pa, sintering procedure is as follows.Manually be warming up to 600 DEG C with 10 DEG C/min, then change time variable control, the temperature rise period: 600 ~ 1800 DEG C, heat-up rate is 10 DEG C/min; Holding stage: 1800 DEG C are incubated 20 hours; Temperature-fall period: 1800 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Tm
0.03y
2.97al
5o
12pottery and Al
2o
3the complex media of monocrystalline puts into hydrogen atmosphere stove anneal, and program is as follows.Temperature rise period: room temperature ~ 1400 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1400 DEG C are incubated 200 hours; Temperature-fall period: 1400 DEG C ~ 700 DEG C, cooling rate is 0.2 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Embodiment 8
By the diameter 10 millimeters of purchase, the Eu of high 1 millimeter
0.02lu
1.98o
3pottery and diameter 10 millimeters, high 1 millimeter of Lu
2o
3crystal carries out light and adds, and requires that the smooth finish of bonding surface is at optics more than three grades, planeness λ/4, f number N=0.5.By two pieces of media after alcohol washes, put into the mixing acid 25 minutes of 15% (sulfuric acid volume: phosphoric acid volume=1:5).Medium is taken out from acid solution, with alcohol washes, then at bonding surface coating 0.35 milliliter, silica gel, carries out gluing, and compress (40 kilograms/cm
2).
The gluing pottery that suppresses and crystalline complex are put into retort furnace and carries out preheating, the water of removing surface adsorption, organism and gas etc.Program is as follows.Temperature rise period: room temperature ~ 300 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 300 DEG C are incubated 5 hours; Temperature rise period: 300 ~ 800 DEG C, heat-up rate is 0.5 DEG C/min; Holding stage: 800 DEG C are incubated 20 hours; Temperature-fall period: 800 DEG C ~ 300 DEG C, cooling rate is 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
By Eu
0.02lu
1.98o
3pottery is put into vacuum sintering furnace with the complex body of monocrystalline and is sintered, and vacuum tightness is 1 × 10
- 5pa, sintering procedure is as follows.Manually be warming up to 600 DEG C with 10 DEG C/min, then change time variable control, the temperature rise period: 600 ~ 1790 DEG C, heat-up rate is 10 DEG C/min; Holding stage: 1790 DEG C are incubated 20 hours; Temperature-fall period: 1790 DEG C ~ 1200 DEG C, cooling rate is 5 DEG C/min; 1200 ~ 700 DEG C, cooling rate is 10 DEG C/min; Less than 700 DEG C Temperature fall are to room temperature.
Finally by Eu
0.02lu
1.98o
3pottery puts into air atmosphere stove anneal with the complex body of monocrystalline, and program is as follows.Temperature rise period: room temperature ~ 1300 DEG C, heat-up rate is 0.2 DEG C/min; Holding stage: 1300 DEG C are incubated 200 hours; Temperature-fall period: 1300 DEG C ~ 700 DEG C, cooling rate is 0.3 DEG C/min; 700 DEG C ~ 300 DEG C, cooling rate is, 1 DEG C/min; Less than 300 DEG C Temperature fall are to room temperature.
Claims (10)
1. a diffusion interlinked method for composite laser medium, is characterized in that comprising the steps:
(1) selection and light add: rare-earth-dopping yttrium aluminum garnet (Re
xy
3-xal
5o
12) laser ceramics, rare earth doped yttrium oxide (Re
xy
2-xo
3) laser ceramics, rear-earth-doped oxidation scandium (Re
xsc
2-xo
3) laser ceramics, rear-earth-doped oxidation lutetium (Re
xlu
2-xo
3) laser ceramics, yttrium aluminum garnet (YAG) pottery, yttrium oxide (Y
2o
3) ceramic, Scium trioxide (Sc
2o
3) ceramic, lutecium oxide (Lu
2o
3) pottery, yttrium aluminum garnet (YAG) crystal, yttrium oxide (Y
2o
3) crystal, Scium trioxide (Sc
2o
3) crystal, lutecium oxide (Lu
2o
3) crystal, sapphire (Al
2o
3), from above-mentioned pottery or crystal, choose two pieces or polylith; Optical manufacturing is carried out again to choosing medium; (2) chemical activation and gluing: by the above-mentioned optics three grades of media that reach after alcohol washes, put into 10% ~ 20%, sulfuric acid volume: phosphoric acid volume=1:5 mixing acid in pickling 10 ~ 40 minutes; Take out peace and quiet, exert pressure with the fixing complex media of molybdenum fixture machinery, add silica gel promote atomic diffusion at medium bonding surface, gluing is complex body; (3) thermal pretreatment: the pottery make gluing clamping pressure or the complex body of crystal are put into muffle furnace and be slowly warmed up to 300 DEG C of insulations 3 ~ 10 hours, slowly be warmed up to 800 DEG C of insulations 20 ~ 60 hours, then slowly room temperature is down to, (4) vacuum high-temperature thermal treatment: complex body is put into vacuum sintering furnace, in vacuum tightness 10
-3~ 10
-5pa, 1600 ~ 1800 DEG C insulation 10 ~ 30 hours, be slowly down to room temperature subsequently; (5) anneal: the complex media obtained is put into atmosphere sintering furnace, under hydrogen, oxygen or air atmosphere, 1200 ~ 1500 DEG C are incubated 40 ~ 200 hours, are down to room temperature subsequently.
2. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: two pieces that choose or polylith medium, Re
xy
3-xal
5o
12, Re
xy
2-xo
3, Re
xsc
2-xo
3, Re
xlu
2-xo
3wherein X is 0.01 ~ 0.6, Re is neodymium (Nd), at least one in erbium (Er), cerium (Ce), holmium (Ho), thulium (Tm), europium (Eu) and chromium (Cr) mixes laser ceramics, and YAG, Y
2o
3, Sc
2o
3, Lu
2o
3, Al
2o
3at least one crystal do not mixed or pottery.
3. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: the smooth finish in conjunction with plane of two pieces or polylith medium reaches optics three grades, planeness λ/4, f number N=0.5.
4. the preparation method of diffusion interlinked composite laser medium according to claim 1, is characterized in that carrying out chemical activation process to dielectric surface, facilitates the atomic diffusion of bonding surface, enhance bond strength.
5. the preparation method of diffusion interlinked composite laser medium according to claim 1, is characterized in that applying a small amount of silica gel by simple method in the conjunction face that medium is tied carries out gluing, utilizes silica gel to promote diffusion interlinked.
6. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: by the complex body of molybdenum clamp pressing two pieces or polylith medium, pressure is at 20 kilograms/cm
2~ 40 kilograms/cm
2between.
7. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: two pieces or polylith medium are same media, or not same media, first medium is carried out successively surface finish, chemical activation, gluing.
8. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: the gluing pottery that suppresses and crystalline complex are put into retort furnace and carried out preheating, the water of removing surface adsorption, organism and gas.
9. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: the complex body being connected with molybdenum fixture is put into the thermal treatment of vacuum oven vacuum high-temperature, in vacuum tightness 10
-3~ 10
-5pa, 1600 ~ 1800 DEG C insulation 10 ~ 30 hours, be slowly down to room temperature subsequently.
10. the diffusion interlinked method of composite laser medium according to claim 1, is characterized in that: composite laser medium is annealed in atmosphere sintering furnace, and under hydrogen, oxygen or air atmosphere, 1200 ~ 1500 DEG C are incubated 40 ~ 200 hours.
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| CN106252206A (en) * | 2016-08-30 | 2016-12-21 | 成都晶九科技有限公司 | Nd:YAG laser crystal large area bonding technology |
| CN106252206B (en) * | 2016-08-30 | 2018-10-19 | 成都晶九科技有限公司 | Nd：YAG laser crystal large area bonding technology |
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