CN1480568A - Method for preparing bonding taser crystal in vertical type with weight applied from top - Google Patents
Method for preparing bonding taser crystal in vertical type with weight applied from top Download PDFInfo
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- CN1480568A CN1480568A CNA031461476A CN03146147A CN1480568A CN 1480568 A CN1480568 A CN 1480568A CN A031461476 A CNA031461476 A CN A031461476A CN 03146147 A CN03146147 A CN 03146147A CN 1480568 A CN1480568 A CN 1480568A
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Abstract
A process for preparing the bonded laser crystical includes vertically overlapping two crystals, applying a weight to at least one crystal, and heat treating.
Description
Technical background
The present invention relates generally to the manufacture method of bonding laser crystals, be specifically related to execute on vertical the method that the bonding laser crystals is made in recasting.
Along with the develop rapidly of science and technology, the laser apparatus particularly demand of solid laser strengthens day by day; And more and more need the large-sized laser crystals of high quality.Yet the preparation of this laser crystals is difficulty relatively, and one needs harsh appointed condition, and two is consuming time expensive.The radius of institute's doping active ions is generally all different with formation crystalline ionic radius in crystal substrate, and this just causes problems of segregation.Large-size crystals particularly, the doping content difference at two ends is big up and down, has a strong impact on the crystalline laser activity.The bonding laser crystals is a new technology, and this technology plays a significant role to the performance of improvement and raising solid laser working substance and laser apparatus thereof.When activating the logical light face of (being mixed with active ions) crystal and/or the non-activation of pump face bonding (undoping) crystal or white stone (Al
2O
3) during crystal, the distortion of operation material heat, the heat effect that cause when improving laser works effectively reduce the wastage and improve laser damage threshold, thereby improve the output rating and the output beam quality of laser apparatus greatly; When crystal bondings such as activation crystal and Q-switch or frequency multiplication, can realize simplifying the structure of laser apparatus from Q-switch or from the output of laser such as frequency multiplication, improve output stability; When high quality activates crystal bonding, can prepare the large size laser bar of high-energy laser, solve the demand of high-energy laser effectively to the large-size high-quality laser bar.For this reason, many countries begin to adopt a kind of method of making the bonding laser crystals, exactly two crystal bondings are become a laser crystals.Make the earliest in this way be Metallic Solids, the someone adopted pressure sintering to prepare halogenide scintillation crystal and semiconductor crystal afterwards; After this develop into oxide crystal.For example EP 0456060 and JP 5255000 disclose a kind of bonding crystalline preparation method, wherein will combine behind two polishing crystals, carefully control heating and cooling repeatedly then and synthesize.JP 59078997 disclosed methods require the atmosphere of heating and cooling.All use tackiness agent or adhering film etc. in the similar approach of many U.S. Patent Publications.Also have and do not use tackiness agent, for example US 5013380, wherein with sapphire rubbing down definite shape, use a kind of anchor clamps combination again, thermal treatment then.Obviously, having relatively high expectations to anchor clamps.US 5441803 discloses a kind of bonding GGG or GSGG crystalline method, wherein connects carrying out light behind two crystal rubbing downs, heats up gradually then and heat-treats.So-called light connects, just the optical cement of China's crystal optics manufacture field; With two respectively crystal carry out optics processing, make at least one end face of each crystal reach certain smooth finish and planeness, with two this end face combinations of crystalline, make it to rely on end face bonded crystal to have certain fastness then.Having relatively high expectations of end face optics processing, narration to some extent in the above-mentioned United States Patent (USP).Also have US5846638 in addition, open bonding doping YAG crystalline method and above chapter are similar.But there are not one piece of patents state or hint in this method, to use weight to be added on the crystal.Only rely on end face in conjunction with to heat-treat then be not enough, one comes the processing of end face optics to be difficult for, two come crystalline size restricted, to than the macrocrystal performance difficulty.So someone proposes to use a kind of precision die in the method, but this Mould Machining difficulty strengthens cost virtually.
Summary of the invention
Therefore, the objective of the invention is to overcome above-mentioned difficulties, a kind of method easy to implement is provided, be a kind of manufacture method of bonding laser crystals, comprise that at least two crystal are carried out light connects thermal treatment then, wherein light is connect the vertical placement of crystal, and at least one crystal, apply weight.
An advantage of the present invention and the high-visible part of a characteristic part will be pointed out hereinafter.
Description of drawings
Accompanying drawing is the synoptic diagram of a preferred embodiment in the inventive method;
DESCRIPTION OF THE PREFERRED
Now referring to accompanying drawing, wherein 1 is the chamber of heat treatment furnace, and 2 and 2 ' is respectively two crystal that light is connected together, the 3rd, and the weight that applies.Can there be many group light to connect crystal and a plurality of weight, 2a and 2 ' a and 3a, 2b and 2 ' b and 3b, 2c and 2 ' c and 3c or the like in the chamber.
Crystal end-face optics processing is well known in the art, carries out crystal end-face that light connects and requires openly in above-mentioned prior art, need not to give unnecessary details.Light connects needs to clean end face as last, removes all contaminations, can be variant according to different its scavenging solutions of crystal.General laser crystals is oxide laser crystal especially, and the mixed solution of the available vitriol oil and 30% hydrogen peroxide cleans, and immerses cleaning liquor then, uses washed with de-ionized water again; Carry out ultrasonic cleaning alternatively, afterwards immediately under environment purification light connect.In addition, make hydrogen bond alternatively before light connects, the present invention preferably makes hydrogen bond.For oxide crystal, the general immersion in the dilute sulphuric acid of pH=1 just can be made hydrogen bond, then the residual sulfuric acid of eccysis.Making hydrogen bond is the known technology of this area equally, need not to give unnecessary details.Key is no matter whether make hydrogen bond, after the cleaning immediately light connect, avoid polluting.Crystal after light connects can be stored under environment purification, waits until thermal treatment.
Owing to apply weight or be called balancing weight in the inventive method, so thermal treatment can be carried out at a lower temperature.The advantage that applies behind the balancing weight not only can reduce thermal treatment temp, and can further reinforce crystalline light and connect, and completely abolishes the use mould.But balancing weight can not be too heavy, otherwise at heat treatment time long slightly or temperature slightly Gao Shihui cause the crystalline stress and strain.Crystalline size and kind not simultaneously, the kind of balancing weight and weight can be variant.Even the phase allomeric but doping content not simultaneously, are compared with identical doping content crystal, the weight of balancing weight is also different.Can draw optimum weight from conventional optimization test, the big or two kinds of crystal doping concentration difference hour weights of general crystal bonding face size, otherwise gentlier; Its scope is preferred 1.0～3.0Kg not mostly.The weight itself that applies is not had strict restriction, if under thermal treatment temp with the crystal reaction and itself do not react not deformation.For simplicity, use, oxide compound or ceramic-like, aluminum oxide for example, titanium dioxide, zirconium dioxide or the like more.
Owing to applied weight, thermal treatment temp generally is lower than the thermal treatment temp of prior art.YAG crystal for example, prior art require to be lower than 1970 ℃ of fusing points, generally about 1800 ℃.And the present invention is lower than 1500 ℃, generally at 1300～1400 ℃.To the crystal of for example GGG, it is enough for 1300 ℃ thermal treatment temp.Even if the ruby that fusing point is higher just can ideally be implemented for maximum 1600 ℃.Temperature is low more, and is just simple more to equipment requirements.As for heat treatment period, there is not strict restriction, as long as obtain the bonding crystal and be not influence laser gain.Because temperature is lower than prior art, the time generally is longer than prior art.During the different crystal different levels of doping, the heat treatment time difference; Big or the doping content difference of crystal bonding face size hour, the time is more longer.These can obtain by conventional optimization test fully, are the conventional meanses of this area.In addition, Equipment for Heating Processing is not had strict restriction equally, no matter resistive heating still be induction heating all can, as long as can reach desired temperature range and try one's best evenly in the heating zone.Particularly than under the long crystal situation, connect part at crystalline light at least and require the temperature uniformity in the zone about 30mm up and down, the thermograde of other parts can not be excessive, is as the criterion not increase crystal stress.These all are known in those skilled in the art.Under the induction heating situation,, can suitably add lagging material for guaranteeing that temperature is even.For example, after crystal light being connect and apply weight, available oxide compound such as aluminum oxide or magnesia powder surround it or the like, thermal treatment afterwards.Warming and cooling rate during thermal treatment does not have strict restriction equally, and condition is not increase bonding crystalline stress.These narrations to some extent in above-mentioned prior art need not to give unnecessary details.
Be described in further detail the present invention below in conjunction with embodiment, certainly, embodiment only limits the present invention absolutely not for explanation.
The low-doped YAG crystal of embodiment 1 bonding
With two YAG (neodymium-doped 1.0at%) crystal end-face polishing of Φ 4 * 60mm, reach light and connect 1: 1 the sulfuric acid (95%) of requirement back immersion and the mixed solution of hydrogen peroxide (30), heating is one hour in about 100 ℃; Immerse cleaning liquor then, use washed with de-ionized water again.The crystal that will clean carries out light and connects in ultra-clean chamber immediately, puts into the resistance High Temperature Furnaces Heating Apparatus.The vertical placement of crystal, the top applies the zirconium white balancing weight of 3.0Kg.Be warmed up to 1300 ℃ with 100 ℃/hour speed, be incubated 50 hours.Drop to room temperature then at the same rate, do not have Tyndall scattering with he-ne laser irradiation crystal bonding face, the result is satisfactory.
The highly doped Y of embodiment 2 bondings
b: the YAG crystal
Y with Φ a 10 * 100mm
b: the YAG crystal end-face polishing of YAG (mixing ytterbium 10at%) crystal and two plain Φ 10 * 10mm, reach light and connect 1: 1 the sulfuric acid (95%) of requirement back immersion and the mixed solution of hydrogen peroxide (30), heating is one hour in about 100 ℃; Immerse cleaning liquor then, add ultrasonic cleaning with deionized water again.Crystal is immersed in the dilute sulphuric acid of pH=1 and make hydrogen bond, put into cleaning liquor-deionized water and ultrasonic cleaning then, in ultra-clean chamber, carry out light immediately and connect, put into medium-frequency induction furnace then.The vertical placement of crystal, the top applies the zirconium white balancing weight of 1.0Kg.Be warmed up to 1300 ℃ with 100 ℃/hour speed, be incubated 40 hours.Drop to room temperature then, detect the crystalline bonding face, the crystal bonding face does not have scattering phenomenon under he-ne laser irradiation, and the result is satisfactory.
Embodiment 3 bonding er-doped E
r: the YAG crystal
Two E with Φ 10 * 50mm
r: the polishing of YAG (er-doped 50at%) crystal end-face, reach light and connect 1: 1 the sulfuric acid (95%) of requirement back immersion and the mixed solution of hydrogen peroxide (30), heating is one hour in about 100 ℃; Immerse cleaning liquor then, add ultrasonic cleaning with deionized water again.Crystal is immersed in the dilute sulphuric acid of pH=1 and make hydrogen bond, put into cleaning liquor-deionized water and ultrasonic cleaning then, in ultra-clean chamber, carry out light immediately and connect, put into medium-frequency induction furnace then.The vertical placement of crystal, the top applies the zirconium white balancing weight of 1.0Kg.Be warmed up to 1300 ℃ with 100 ℃/hour speed, be incubated 35 hours.Drop to room temperature then, do not have scattering phenomenon with he-ne laser irradiation crystal bonding face, the result is satisfactory.
Embodiment 4 bonding titanium gem crystals
Two T with 6mm * 12mm
i: Al
2O
3The polishing of (mixing titanium 0.3at%) crystal end-face reaches light and connects 1: 1 the sulfuric acid (95%) of requirement back immersion and the mixed solution of hydrogen peroxide (30), and heating is one hour in about 100 ℃; Immerse cleaning liquor then, add ultrasonic cleaning with deionized water again.Crystal is immersed in the dilute sulphuric acid of pH=1 and make hydrogen bond, put into cleaning liquor-deionized water and ultrasonic cleaning then, in ultra-clean chamber, carry out light immediately and connect, put into medium-frequency induction furnace then.The vertical placement of crystal, the top applies the zirconium white balancing weight of 3.0Kg.Be warmed up to 1400 ℃ with 100 ℃/hour speed, be incubated 60 hours.Drop to room temperature then, do not have scattering phenomenon with helium-neon laser irradiation crystal bonding face, the result is satisfactory.
Embodiment more than 5 group bondings mix, and YAG and titanium gem crystal undope
With the class of operation of embodiment 2 seemingly, different is:
T
i: Al
2O
3+ YAG+N
d: YAG+YAG+T
i: Al
2O
3Size be respectively execute on 5 * 6mm * 12mm. accompany heavy 3.0 kilograms.
The present invention has been described in detail in detail above, and obviously, those skilled in the art can do many variations and improvement and not deviate from spiritual scope of the present invention.
Claims (11)
1. the manufacture method of a bonding laser crystals comprises that at least two crystal are carried out light to be connect, and thermal treatment then is characterized in that light is connect the vertical placement of crystal, and apply weight at least one crystal.
2. according to the method for claim 1, it is characterized in that light connects further to be included in crystal end-face and to make hydrogen bond.
3. according to the method for claim 2, it is characterized in that making hydrogen bond is to carry out in the dilute sulphuric acid of pH=1.
4. according to the method for claim 1, it is characterized in that applying weight of heavy between 1.0～3.0Kg.
5. according to the method for claim 1, it is characterized in that crystal is to mix or the yttrium aluminum garnet that undopes (YAG) crystal.
6. according to the method for claim 1, it is characterized in that crystal is titanium jewel T
i: AI
2O
3Or sapphire AI
2O
3Crystal.
7. according to the method for claim 1, it is characterized in that it is to mix or one in the YAG crystal that undopes mixes or undopes AI that light connects one in crystal
2O
3Crystal.
8. according to the method for claim 1, it is characterized in that crystal is to mix or the yttrium aluminate that undopes (YAP) crystal.
9. according to the method for claim 1, it is characterized in that crystal is to mix or the GGG crystal that undopes.
10. according to the method for claim 1, it is characterized in that Equipment for Heating Processing is a resistance heading furnace.
11., it is characterized in that Equipment for Heating Processing is an induction heater according to the method for claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031461476A CN1480568A (en) | 2003-07-24 | 2003-07-24 | Method for preparing bonding taser crystal in vertical type with weight applied from top |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031461476A CN1480568A (en) | 2003-07-24 | 2003-07-24 | Method for preparing bonding taser crystal in vertical type with weight applied from top |
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|---|---|
| CN1480568A true CN1480568A (en) | 2004-03-10 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436966A (en) * | 2013-08-13 | 2013-12-11 | 安徽环巢光电科技有限公司 | Method for bonding doped or pure yttrium aluminum garnet crystal and doped yttrium aluminum garnet crystal by molten salt method |
| CN106087055A (en) * | 2016-06-15 | 2016-11-09 | 北京雷生强式科技有限责任公司 | A kind of yttrium aluminate composite crystal and preparation method thereof |
| CN107964683A (en) * | 2017-11-28 | 2018-04-27 | 北京雷生强式科技有限责任公司 | The thermal bonding method and device of laser crystal |
| WO2021208363A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Device for preparing large-size single crystal |
-
2003
- 2003-07-24 CN CNA031461476A patent/CN1480568A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436966A (en) * | 2013-08-13 | 2013-12-11 | 安徽环巢光电科技有限公司 | Method for bonding doped or pure yttrium aluminum garnet crystal and doped yttrium aluminum garnet crystal by molten salt method |
| CN103436966B (en) * | 2013-08-13 | 2016-05-04 | 安徽环巢光电科技有限公司 | The method of the doping of molten-salt growth method bonding or pure yttrium-aluminium-garnet and doped yttrium aluminum garnet crystal |
| CN106087055A (en) * | 2016-06-15 | 2016-11-09 | 北京雷生强式科技有限责任公司 | A kind of yttrium aluminate composite crystal and preparation method thereof |
| CN107964683A (en) * | 2017-11-28 | 2018-04-27 | 北京雷生强式科技有限责任公司 | The thermal bonding method and device of laser crystal |
| WO2021208363A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Device for preparing large-size single crystal |
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