CN106192010A - A kind of manufacture method of nonlinear crystal gallium selenide components and parts - Google Patents
A kind of manufacture method of nonlinear crystal gallium selenide components and parts Download PDFInfo
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- CN106192010A CN106192010A CN201610669688.1A CN201610669688A CN106192010A CN 106192010 A CN106192010 A CN 106192010A CN 201610669688 A CN201610669688 A CN 201610669688A CN 106192010 A CN106192010 A CN 106192010A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The manufacture method of a kind of nonlinear crystal gallium selenide components and parts, the present invention relates to the manufacture method of crystal element and device.The present invention is to solve the technical problem that existing GaSe crystal transmitance is low and the most yielding, cleave.This method: one, by cleaning, drying after GaSe crystal ingot surface etch；Two, crystal ingot is put in bateau, then bateau is put in the middle part of quartz ampoule, place GaSe polycrystal powder at bateau two ends；Or putting GaSe polycrystal powder in bateau one end, the other end puts Se；To sealing by fusing after quartz ampoule evacuation, put in mono temperature area resistance furnace；Three, annealing；Four, by crystal ingot cutting after annealing and it is trimmed to GaSe crystal block along c-axis direction；Five, GaSe crystal block glue being fixed on the position of the hole of metab, puts politef overcoat, add upper cover, then coupled together with upper cover by base with fixing nut, obtaining GaSe components and parts, this device can be used in laser instrument.
Description
Technical field
The present invention relates to the manufacture method of crystal element and device.
Background technology
Gallium selenide (GaSe) crystal has that nonlinear factor is big, transmission region width, birefringence big, laser damage threshold relatively
High and be perpendicular to optical axis direction thermal conductivity advantages of higher, it is the most important and best material producing 8-10 μm mid and far infrared laser
One of.GaSe crystal can realize the power output of terahertz wave band, and it is at 0.1 10.0THz wave band linear optics absorptance
It is that current terahertz wave band nonlinear optical crystal absorbs minimum.GaSe is hexagonal layered crystal, space groupLattice paprmeter a=0.375nm, c=1.595nm, each layer is tied by covalent bond mutually by the order of Se-Ga-Ga-Se
Closing, wherein Ga-Ga key is parallel to c-axis, is combined by Van der Waals force between layers.GaSe crystal is being perpendicular to c-axis direction
Easily cleaving, relative hardness is almost nil, and therefore it the most easily deforms.Additionally this crystal is at synthesised polycrystalline raw material
Stage and crystal growth stage, the non-stoichiometric caused due to component volatilization, it is easily formed point defect, dislocation and inclusion enclave
Deng, reduce the transmitance of this crystal, reduce serviceability.
Summary of the invention
The present invention is to solve that existing GaSe crystal transmitance technology low and the most yielding, splitting is asked
Topic, and the manufacture method of a kind of nonlinear crystal GaSe components and parts is provided.
The manufacture method of the nonlinear crystal GaSe components and parts of the present invention, sequentially includes the following steps:
One, volume ratio HCl:HNO is used3=1:(3～3.5) nitration mixture to GaSe crystal ingot surface etch 1～2 minutes, with
Remove the impurity such as plane of crystal oxide, then clean with ultra-pure water, dry；
Two, GaSe crystal ingot is put in quartz bateau or boron nitride (PBN) bateau, then bateau is put in the middle part of quartz ampoule；
Place GaSe polycrystal powder at bateau two ends, crystal ingot is 10:(1～2 with the mass ratio of polycrystal powder)；Or put in one end of bateau
GaSe polycrystal powder, it is 10:(0.5～1 that the other end puts the mass ratio of simple substance Se, crystal ingot and polycrystal powder), crystal ingot and the matter of Se
Amount ratio is 10:(0.05～0.1)；Then quartz ampoule is evacuated to 10-4～10-6Pa, with oxyhydrogen flame sealing by fusing quartz ampoule, puts
Enter in mono temperature area resistance furnace；
Three, resistance furnace is warming up to 450 DEG C～500 DEG C, is incubated 100h～150h, then with 20 DEG C～25 DEG C/h rate of temperature fall
It is cooled to room temperature, obtains crystal ingot of annealing；
Four, annealing crystal ingot is dissociated into nature smooth flat along being perpendicular to c-axis (optical axis) direction, and this is the most smooth flat
Face is fixed on cutter supporting frame panel, is then cut into square block, and edge is perpendicular to c-axis direction and is trimmed to GaSe crystalline substance the most again
Body block；
Five, getting out base, upper cover, politef overcoat and fixing nut, wherein the material of base and upper cover is gold
Belong to, hole is set in the middle of base with upper cover, GaSe crystal block glue is fixed on the position of the hole of base, puts polytetrafluoro
Ethylene overcoat, adds upper cover, then is coupled together with upper cover by base with fixing nut, obtain nonlinear crystal GaSe components and parts.
The GaSe crystal block used by GaSe components and parts of the present invention makes annealing treatment before cutting, not only may be used by annealing
To eliminate the thermal stress formed when crystal growth, and when annealed crystal is in the steam atmosphere of GaSe and is incubated long enough
Time, part Ga and Se atom can be diffused into crystals by plane of crystal, compensate the atom of disappearance in lattice, eliminate point
Defect, corrects dislocation simultaneously, reduces defect concentrations in crystals, improves transmitance.The GaSe components and parts of the present invention by metallic aluminium (or
Copper) and the material such as politef make shell, not only can effectively fix crystal, protection crystal is not damaged by external force
Evil, and directly metab and the upper cover on the contact upper and lower surface of crystal can increase crystal radiating surface in use
Long-pending, reduce thermal lensing effect, improve crystal serviceability, stability and life-span.
Accompanying drawing explanation
Fig. 1 is the position view that in embodiment 1, in step 2, GaSe crystal ingot is put in quartz ampoule；In figure, 1 is that GaSe is brilliant
Ingot, 2 is bateau, and 3 is quartz ampoule, and 4 is GaSe polycrystal powder or Se raw material；
Fig. 2 is the structural representation of GaSe components and parts in embodiment 1；In figure, 5 is gallium selenide crystal wafer, and 6 is metal top cover,
8 is politef overcoat, and 9 is fixing nut；
Fig. 3 is the structural profile schematic diagram of GaSe components and parts in embodiment 1；In figure, 7 is base；
Fig. 4 is the photo of GaSe components and parts in embodiment 1；
Fig. 5 be in embodiment 1 GaSe crystal block annealing before and after Transmittance spectrum；
Fig. 6 is the terahertz wave band absorptance spectrogram of GaSe components and parts in embodiment 1.
Detailed description of the invention
Detailed description of the invention one: the manufacture method of the nonlinear crystal GaSe components and parts of present embodiment, according to the following steps
Carry out:
One, volume ratio HCl:HNO is used3=1:(3～3.5) nitration mixture to GaSe crystal ingot surface etch 1～2 minutes, with
Remove the impurity such as plane of crystal oxide, then clean with ultra-pure water, dry；
Two, GaSe crystal ingot is put in quartz bateau or boron nitride (PBN) bateau, then bateau is put in the middle part of quartz ampoule；
Place GaSe polycrystal powder at bateau two ends, crystal ingot is 10:(1～2 with the mass ratio of polycrystal powder)；Or put in one end of bateau
GaSe polycrystal powder, it is 10:(0.5～1 that the other end puts the mass ratio of simple substance Se, crystal ingot and polycrystal powder), crystal ingot and the matter of Se
Amount ratio is 10:(0.05～0.1)；Then quartz ampoule is evacuated to 10-4～10-6Pa, with oxyhydrogen flame sealing by fusing quartz ampoule, puts
Enter in mono temperature area resistance furnace；
Three, resistance furnace is warming up to 450 DEG C～500 DEG C, is incubated 100h～150h, then with 20 DEG C～25 DEG C/h rate of temperature fall
It is cooled to room temperature, obtains crystal ingot of annealing；
Four, annealing crystal ingot is dissociated into nature smooth flat along being perpendicular to c-axis (optical axis) direction, and this is the most smooth flat
Face is fixed on cutter supporting frame panel, is then cut into square block, and edge is perpendicular to c-axis direction and is trimmed to GaSe crystalline substance the most again
Body block；
Five, base 7, upper cover 6, politef overcoat 8 and fixing nut 9, wherein base 7 and the material of upper cover 6 are got out
Material is metal, arranges hole, GaSe crystal block glue is fixed on the position of the hole of base in the middle of base 7 with upper cover 6, set
Upper politef overcoat 8, adds upper cover 6, is coupled together with upper cover 6 by base 7 with fixing nut 9, obtains non-linear crystalline substance
Body GaSe components and parts.
Detailed description of the invention two: the drying temperature in present embodiment step one unlike detailed description of the invention one is
50 DEG C～60 DEG C.Other is identical with detailed description of the invention one.
Detailed description of the invention three: the quartz ampoule in present embodiment step one unlike detailed description of the invention one or two
It is evacuated to 10-4～10-6Pa.Other is identical with detailed description of the invention one or two.
Detailed description of the invention four: resistance in present embodiment step 3 unlike one of detailed description of the invention one to three
The heating rate of stove is 40～60 DEG C/h.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: anneal in present embodiment step 3 unlike one of detailed description of the invention one to four
Temperature is 470 DEG C～480 DEG C.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: resistance in present embodiment step 3 unlike one of detailed description of the invention one to five
The rate of temperature fall of stove is 20 DEG C～25 DEG C/h.Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: GaSe in present embodiment step 4 unlike one of detailed description of the invention one to six
The thickness of crystal block is 10mm～15mm.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: in present embodiment step 5 unlike one of detailed description of the invention one to seven, Gu
The glue determined is PUR or UV glue.Other is identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: in present embodiment step 5 unlike one of detailed description of the invention one to eight, the end
The material of seat and upper cover is aluminum or copper.Other is identical with one of detailed description of the invention one to eight.
Beneficial effects of the present invention is verified by following example:
Embodiment 1, the manufacture method of nonlinear crystal gallium selenide components and parts of the present embodiment, sequentially include the following steps:
One, volume ratio HCl:HNO is used3The nitration mixture of=1: 3 was to GaSe crystal ingot surface etch 1 minute, to remove crystal table
The impurity such as face oxide, then clean, in 50 DEG C of drying with ultra-pure water；
Two, GaSe crystal ingot 1 is put in PBN bateau 2, then bateau is put in the middle part of quartz ampoule 3, place at bateau two ends
GaSe polycrystal powder 4, crystal ingot 1 is 10: 2 with the mass ratio of polycrystal powder 4；Quartz ampoule 3 is evacuated to 10-5Pa, with hydrogen-oxygen fire
Flame sealing by fusing quartz ampoule 3, puts in mono temperature area resistance furnace；This step GaSe crystal ingot puts into the such as Fig. 1 of the position view in quartz ampoule
Shown in；
Three, resistance furnace is warming up to 480 DEG C with 50 DEG C/h heating rate, is incubated 120h, then drops with 25 DEG C/h rate of temperature fall
Warm to room temperature, the annealing crystal ingot obtained；
Four, annealing crystal ingot is dissociated into nature smooth flat along being perpendicular to c-axis direction, and this natural smooth flat is fixed
On cutter supporting frame panel, being then cut into 13mm × 13mm square block, edge is perpendicular to c-axis direction and is trimmed to thickness the most again
Degree is the GaSe crystal wafer of 10mm；Due to this crystal dynamics poor-performing, it is not suitable for being processed by shot blasting, so at finishing crystal
During thickness, need to ensure that transparent surface (face of dissociating) is nature smooth flat；
Five, GaSe components and parts are by GaSe crystal wafer 5, upper cover 6, base 7, politef overcoat 8 and 9 groups of fixing nut
Becoming, wherein base 7 and upper cover 6 are diameter 50mm, thickness 2mm circle aluminium flake, arrange a diameter of in the middle of base with upper cover
The circular hole of 12mm, base has external screw thread, width of thread 1mm with the side car of upper cover；Politef overcoat be internal diameter be 50mm,
The cylinder of wall thickness 1mm, highly 14mm；GaSe crystal wafer is put on the circular hole of base, and crystal c axle is perpendicular to aluminium flake, thoroughly
Bright finish is parallel with aluminium flake, and light can be along being perpendicular to crystal layer direction, and in the middle of aluminium flake, circular hole passes through, crystal wafer 5 surrounding heat
Melten gel is fixed on base, is connected with fixing nut between base with upper cover.The structural representation of these GaSe components and parts such as Fig. 2 institute
Showing, profile is as shown in Figure 3.
The photo of GaSe components and parts prepared by the present embodiment as shown in Figure 4, device diameters 50mm, center-hole diameter 12mm.
Fig. 5 is Transmittance spectrum before and after the annealing of 10mm thickness GaSe crystal block, crystal transmitance phase after data display annealing in figure
Significantly improve than transmitance before annealing.
Fig. 6 is by the room temperature GaSe terahertz wave band absorptance spectrum of terahertz time-domain spectroscopy system test, it can be seen that
At 0.1～1.5THz wave band, except there being a sharp-pointed absworption peak at 0.6THz, remaining wave band Terahertz absorbs more weak, less than 5cm-1。
Claims (9)
1. the manufacture method of nonlinear crystal GaSe components and parts, it is characterised in that this manufacture method sequentially includes the following steps:
One, volume ratio HCl:HNO is used3=1:(3～3.5) nitration mixture to GaSe crystal ingot surface etch 1～2 minutes, then with super
Pure water cleans, dries；
Two, GaSe crystal ingot is put in quartz bateau or boron nitride bateau, then bateau is put in the middle part of quartz ampoule；At bateau two ends
Placing GaSe polycrystal powder, crystal ingot is 10:(1～2 with the mass ratio of polycrystal powder)；Or put GaSe polycrystal powder in one end of bateau
End, it is 10:(0.5～1 that the other end puts the mass ratio of simple substance Se, crystal ingot and polycrystal powder), crystal ingot is 10 with the mass ratio of Se:
(0.05～0.1)；Then quartz ampoule is evacuated to 10-4～10-6Pa, with oxyhydrogen flame sealing by fusing quartz ampoule, puts into single warm area
In resistance furnace；
Three, resistance furnace is warming up to 450 DEG C～500 DEG C, is incubated 100h～150h, then with 20 DEG C～25 DEG C/h rate of temperature fall coolings
To room temperature, obtain crystal ingot of annealing；
Four, annealing crystal ingot is dissociated into nature smooth flat along being perpendicular to c-axis direction, and this natural smooth flat is fixed on cuts
On cutting mill support panel, being then cut into square block, edge is perpendicular to c-axis direction and is trimmed to crystal block the most again；
Five, base (7), upper cover (6), politef overcoat (8) and fixing nut (9), wherein base (7) and upper cover are got out
(6) material is metal, arranges hole, GaSe crystal block glue is fixed on the hole of base in the middle of base (7) with upper cover (6)
The position in hole, puts politef overcoat (8), adds upper cover (6), then with fixing nut (9) by base (7) and upper cover (6)
Couple together, obtain nonlinear crystal GaSe components and parts.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1, it is characterised in that step one
In drying temperature be 50 DEG C～60 DEG C.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
Quartz ampoule in one is evacuated to 10-4～10-6Pa.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
In three, the heating rate of resistance furnace is 40～60 DEG C/h.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
In three, annealing temperature is 470 DEG C～480 DEG C.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
In three, the rate of temperature fall of resistance furnace is 20 DEG C～25 DEG C/h.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
In four, the thickness of GaSe crystal block is 10mm～15mm.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
In five, fixing glue is PUR or UV glue.
The manufacture method of a kind of nonlinear crystal GaSe components and parts the most according to claim 1 and 2, it is characterised in that step
In five, the material of base (7) and upper cover (6) is aluminum or copper.
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| CN201610669688.1A CN106192010B (en) | 2016-08-15 | 2016-08-15 | A kind of production method of nonlinear crystal gallium selenide component |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050139147A1 (en) * | 2003-12-30 | 2005-06-30 | Liming Wang | Method for annealing group IIA metal fluoride crystals |
| CN102409407A (en) * | 2011-11-09 | 2012-04-11 | 中国科学院福建物质结构研究所 | Infrared non-linear optical material Ba3AGa5Se10Cl2 and preparation method thereof |
| CN105755542A (en) * | 2016-05-12 | 2016-07-13 | 中国科学院福建物质结构研究所 | Crystal material, preparation method of crystal material, and application of crystal material as non-linear optical crystal |
| CN105803531A (en) * | 2016-04-13 | 2016-07-27 | 浙江大学 | Four-element selenide non-linear optical crystal and preparing method and application thereof |
-
2016
- 2016-08-15 CN CN201610669688.1A patent/CN106192010B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050139147A1 (en) * | 2003-12-30 | 2005-06-30 | Liming Wang | Method for annealing group IIA metal fluoride crystals |
| CN102409407A (en) * | 2011-11-09 | 2012-04-11 | 中国科学院福建物质结构研究所 | Infrared non-linear optical material Ba3AGa5Se10Cl2 and preparation method thereof |
| CN105803531A (en) * | 2016-04-13 | 2016-07-27 | 浙江大学 | Four-element selenide non-linear optical crystal and preparing method and application thereof |
| CN105755542A (en) * | 2016-05-12 | 2016-07-13 | 中国科学院福建物质结构研究所 | Crystal material, preparation method of crystal material, and application of crystal material as non-linear optical crystal |
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| CN106192010B (en) | 2018-10-26 |
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