CN102703983A - Method and device for compressing free space in cadmium zinc telluride crystal growing crucible through double sealing sleeves - Google Patents
Method and device for compressing free space in cadmium zinc telluride crystal growing crucible through double sealing sleeves Download PDFInfo
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- CN102703983A CN102703983A CN2012101969259A CN201210196925A CN102703983A CN 102703983 A CN102703983 A CN 102703983A CN 2012101969259 A CN2012101969259 A CN 2012101969259A CN 201210196925 A CN201210196925 A CN 201210196925A CN 102703983 A CN102703983 A CN 102703983A
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Abstract
The invention relates to a method and a device for compressing a free space in a cadmium zinc telluride crystal growing crucible through double sealing sleeves and belongs to the technical field of special crystal growth. The method has the main technical scheme that Cd, Zn and Te raw materials which meet Cd1-xZnxTe (x is 0.04 to 0.8) and have the purity being 99.99999 percent are charged into a quartz crucible, a secondary sealing sleeve and a primary sealing sleeve are sequentially placed into the quartz crucible, the vacuum pumping is carried out until the pressure is 2.0*10<-4>Pa, and the quartz crucible is sealed and knotted at the primary sealing sleeve part. The sealed crucible is placed into a material blending furnace, the temperature is slowly raised to 500 DEG C, after the heat insulation for a certain time, the temperature is slowly raised, and the material blending and the heat insulation are carried out after the melting point of materials is reached. The temperature is slowly lowered to the room temperature, and the material blending is completed. Then, the crucible is taken out, the crucible is subjected to secondary pipe sealing at the secondary sealing sleeve part. The primary sealing sleeve part at the tail part is cut off, and the crucible containing CdZnTe materials is placed into a crystal growth furnace for carrying out single crystal growth. The size compression on the free space during the crystal growth is realized through using the double sealing sleeves by the secondary pipe sealing method, and in the subsequent single crystal growth process, the formation of Cd vacant sites in crystals can be effectively inhibited, so the performance of the crystals is improved.
Description
Technical field
The method and apparatus of free space volumes belongs to special crystal growth technique technical field in the quartz crucible when the present invention relates to two big envelopes of a kind of employing and reducing the CdZnTe crystal growth through twice closed quartz tube with this.
Background technology
Tellurium zinc cadmium Cd
1-xZn
xTe (CZT) is a kind of semiconductor material with wide application prospect, and the preparation of its body monocrystalline gets more and more people's extensive concerning always.Because its energy gap energy gap of CdZnTe (CZT) single crystal big (Eg=1.70eV), staple Cd, the Te ordination number is high, resistivity is high by (10
11Ω cm), the big (μ of electronics and void migration rate
e=1100cm/Vs, μ
h=100cm/Vs), wide (10keV～6MeV), energy resolution are high, anti-neutron and proton irradiation damage threshold are also higher for the energy investigative range; So the CdZnTe detector has bigger uptake factor, higher CR; Especially do not need any cooling apparatus just can at room temperature work, thereby volume is less, it is convenient to use.
But the generation difficulty of CdZnTe single crystal itself is big, and crystal mass is difficult to reach the industrial standards of general commercial user for the components and parts customization usually.At present, the widespread use of CdZnTe detector mainly receives the restriction of several respects such as crystal property, volume and cost, wherein the crystalline self-defect to the big limitations of influence of crystal property the development of CdZnTe detector.
Wherein influence one of crystal property very important reasons be to be the non-congruent boiling characteristics of CdZnTe crystalline; Especially because the high-vapor-pressure characteristic of Cd; Make that in crystal growing process a large amount of Cd escapes in the freeboard in the crucible from the crystal of melt and high growth temperature attitude, exist a large amount of Cd rooms in the crystal that causes growth to accomplish; And the existence in a large amount of Cd rooms can reduce resistivity; Have in crystal, mix In again with compensation Cd room in order to improve resistivity, and improve the carrier lifetime product that resistivity can reduce material through compensation way, the result has influenced crystalline power spectrum response characteristic; So the problems referred to above do not solve, even cause adopting highly purified starting material to be difficult to grow high performance crystal yet.Therefore, how reducing the generation in Cd room through the improvement crystal growth technique, further promote crystal property, is to obtain high quality CdZnTe crystalline essential condition.
In present growth technique, generally reduce Cd double-void CdZnTe crystalline disadvantageous effect through methods such as doped shallow donor impurity (elements such as Al, In, Cl) compensation Cd room, rich Cd batching minimizing Cd rooms.But when doped shallow donor impurity compensation Cd room, the concentration in shallow donor impurity and Cd room is difficult to accomplish that about equally the essential deep energy level of introducing is come " pinning " residue shallow energy level.But deep energy level is trap and deathnium, and the deep energy level density of introducing is excessive, will greatly reduce μ τ (product of carrier lifetime and mobility) value.And can reduce CdZnTe crystalline quality and performance because of the reason of rich Cd growth through the method in rich Cd batching minimizing Cd room.Therefore, seeking the further concentration that reduces Cd room in the crystal of a kind of new process modification method is further to promote crystal mass to obtain to have high resolving power ability spectrum level crystalline important channel.
A kind of feasible thinking is to limit the concentration in Cd room through reducing the freeboard that in crystal growing process, can supply the Cd component to overflow.In crystal growing process, the component in the CdZnTe material is overflowed to the freeboard of crystal top at a certain temperature.Because the vp of Cd is bigger among the CdZnTe, in freeboard, Cd steam has accounted for major part, ubiquity Cd room in the CdZnTe crystal that obtains that causes growing.Therefore the volume that reduces freeboard is an important channel that effectively suppresses Cd vacancy concentration in the CdZnTe crystal.
Summary of the invention
The technical problem that the present invention will solve: the present invention is the method and the device thereof of Cd vacancy concentration in a kind of CdZnTe of minimizing crystal.The present invention can significantly reduce the freeboard in the quartz crucible when the CdZnTe single crystal growing, at high temperature cause more Cd component to escape into the problem that freeboard forms steam owing to the Cd dividing potential drop is higher thereby solve.The Cd room of adopting the present invention to grow in the CdZnTe crystal of gained significantly reduces, and has improved crystal property.
The method and apparatus that the purpose of this invention is to provide freeboard in a kind of pair of big envelope compression growing tellurium zinc cadmium crystal crucible.
1. the method for freeboard in two big envelopes compression growing tellurium zinc cadmium crystal crucibles is characterized in that having following technological process and step:
A. according to required proportioning high-purity Cd, Zn, Te raw material are packed in the high-purity silica pot earlier, successively put into secondary big envelope and a big envelope then, the secondary big envelope is positioned at the material top, and one time big envelope is positioned at secondary big envelope top; Quartz crucible is evacuated to 2.0 * 10
-4Pa under this vacuum tightness, carries out tube sealing at a big envelope place No. one time to quartz crucible;
B. the quartz crucible of sealing is put into and waved stove and close material, be warming up to 500 ℃, be incubated, be warming up to slowly then and close 1130 ℃ ~ 1140 ℃ of material temperature, insulation 24 ~ 40h is cooled to room temperature subsequently slowly, obtain the CdZnTe polycrystalline after, close material and finish; The secondary big envelope is close to the top of gained polycrystal owing to the self gravitation effect at this moment;
C. with above-mentioned close quartz crucible that material finishes and take out after, the place carries out the secondary tube sealing in the secondary big envelope, cut the part of a big envelope of afterbody then after, put into crystal growing furnace and carry out the growth of CdZnTe crystalline; The single crystal growing temperature is 1115 ℃; Under such processing condition; The volume of the freeboard of polycrystal top is limited in alap level; Thereby when follow-up crystal growth, reduced the concentration in the Cd room that in crystal, produces because the Cd vp is big, improved CdZnTe crystalline performance.
2. the used device of method of freeboard in two big envelopes compression growing tellurium zinc cadmium crystal crucibles, this device is made up of high-purity silica pot (1), a big envelope (2), secondary big envelope (3); It is characterized in that: a big envelope (2) is positioned at secondary big envelope (3) top, and secondary big envelope (3) can freely move up and down in quartz crucible (1); Closing the material front and back, secondary big envelope (3) can be close to the tellurium zinc cadmium material top in the crucible.
The characteristics of the inventive method are different with commonly used quartz crucible tube sealing method of past:
The quartz crucible tube sealing method of single big envelope was under the situation of guaranteeing the certain vacuum degree, at the quartz crucible top quartz crucible to be carried out tube sealing and closes material in the past; So just between CdZnTe material and big envelope, stayed more a certain amount of freeboard; In single crystal growth process; Cd component in the material is overflowed to freeboard, and this generation for the Cd room has direct influence.And utilize two big envelopes to realize the compression of freeboard through secondary pipe sealing method and minimize, make that in follow-up single crystal growth process freeboard is farthest limited for the influence of Cd vacancy concentration.
Description of drawings
Fig. 1 is for utilizing two twice tube sealing of big envelope method and device synoptic diagram of free space volumes in the quartz crucible when reducing the CdZnTe crystal growth; Wherein Fig. 1 (a) is the view of closing behind tube sealing before the material, the synoptic diagram when Fig. 1 (b) carries out the secondary tube sealing for closing behind the material.
Embodiment
Embodiment one:
Referring to Fig. 1, used device comprises high-purity silica pot 1, big envelope 2, secondary big envelope 3 among the present invention; One time big envelope 2 is positioned at secondary big envelope 3 tops, and secondary big envelope 3 can freely move up and down in quartz crucible 1.A big envelope 2 is the high purity quartz big envelope of one section opening of a hollow, and secondary big envelope 3 is a hollow circular cylinder high purity quartz big envelope, the inner certain vacuum degree that keeps.Closing the material front and back, secondary big envelope 3 can be close to the CdZnTe material in the crucible.
The concrete process step method of present embodiment is described below:
1) will satisfy Cd
1-xZn
xThe purity of Te (x=0.04～0.8) is that 99.99999% high-purity Cd, Zn, Te raw material are packed in the high-purity silica pot, puts into two quartz envelope successively, and is evacuated to 2.0 * 10
-4Pa uses oxyhydrogen flame with the big envelope outside and inner wall of quartz crucible sealing by fusing (closed quartz tube for the first time).
2) polycrystalline of CdZnTe closes material and all in above-mentioned same high-purity silica pot, carries out with growing single-crystal growth in this growth method, has so just reduced the possibility of the detrimental impurity of secondary replace tubes charging introducing.The above-mentioned quartz crucible of sealing put into close the material stove, slowly be warming up to about 500 ℃,, slowly be warming up to and close the material insulation more than the material fusing point through after the insulation of certain hour.Cd
1-xZn
xThe fusing point of Te changes according to the difference of x value.When x=0.04, fusing point is 1095 ℃; When x=0.1, fusing point is 1115 ℃; Fusing point is 1130 ℃ when x=0.2.For guaranteeing that closing material fully accomplishes, will close the material temperature and be made as about 1140 ℃.In the process of insulation, shake quartz crucible, make material reaction complete.Slowly be cooled to room temperature subsequently, polycrystalline closes the material end of processing.
3) quartz crucible is taken out from close the material stove.At this moment; The CdZnTe polycrystal is positioned at the quartz crucible bottom; And another big envelope of before a tube sealing, putting in advance (being the secondary big envelope) can freely move up and down at crucible, lets this big envelope under the self gravitation effect, is close to CdZnTe polycrystal top; And reuse oxyhydrogen flame and utilize this big envelope that quartz crucible is carried out secondary tube sealing (for the second time closed quartz tube), then the freeboard of CdZnTe polycrystal top has just obtained compression to greatest extent.Cut big envelope part of afterbody; The quartz crucible that the CdZnTe polycrystal is housed is put into the growth that crystal growing furnace carries out monocrystalline.The temperature of single crystal growing is 1115 ℃.
Embodiment two:
Present embodiment adopts same growing apparatus in the foregoing description one.
Growth technique step and the foregoing description one in the present embodiment are identical, and different is to have changed some processing parameters.Its different parameter is: changed closing when closing material and expected temperature and soaking time, be respectively 1135 ℃ and 40h.
Adopt the apparatus and method of free space volumes in the two big envelope compression of the utilization of the present invention quartz crucible, Stability Analysis of Structures, simple to operate, repeatable strong.The volume of the freeboard in the time of can effectively reducing the CdZnTe single crystal growing through technology of the present invention in the quartz crucible; Cd vacancy concentration in the CdZnTe monocrystalline that restriction obtains; Material and the long brilliant contaminating impurity that the secondary charging possibly introduced that separates have also been avoided simultaneously closing; Finally can obtain high quality, highly purified CdZnTe crystal, meet requirement fully as material for detector.
Claims (2)
1. the method for freeboard in two big envelopes compression growing tellurium zinc cadmium crystal crucibles is characterized in that having following technological process and step:
A. according to required proportioning high-purity Cd, Zn, Te raw material are packed in the high-purity silica pot earlier, successively put into secondary big envelope and a big envelope then, the secondary big envelope is positioned at the material top, and one time big envelope is positioned at secondary big envelope top; Quartz crucible is evacuated to 2.0 * 10
-4Pa under this vacuum tightness, carries out tube sealing at a big envelope place No. one time to quartz crucible;
B. the quartz crucible of sealing is put into and waved stove and close material, be warming up to 500 ℃, be incubated, be warming up to slowly then and close 1130 ℃ ~ 1140 ℃ of material temperature, insulation 24 ~ 40h is cooled to room temperature subsequently slowly, obtain the CdZnTe polycrystalline after, close material and finish; The secondary big envelope is close to the top of gained polycrystal owing to the self gravitation effect at this moment;
C. with above-mentioned close quartz crucible that material finishes and take out after, the place carries out the secondary tube sealing in the secondary big envelope, cut the part of a big envelope of afterbody then after, put into crystal growing furnace and carry out the growth of CdZnTe crystalline; The single crystal growing temperature is 1115 ℃; Under such processing condition; The volume of the freeboard of polycrystal top is limited in alap level; Thereby when follow-up crystal growth, reduced the concentration in the Cd room that in crystal, produces because the Cd vp is big, improved CdZnTe crystalline performance.
2. the used device of method of freeboard in two big envelopes compression growing tellurium zinc cadmium crystal crucibles, this device is made up of high-purity silica pot (1), a big envelope (2), secondary big envelope (3); It is characterized in that: a big envelope (2) is positioned at secondary big envelope (3) top, and secondary big envelope (3) can freely move up and down in quartz crucible (1); Closing the material front and back, secondary big envelope (3) can be close to the tellurium zinc cadmium material top in the crucible.
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| CN2012101969259A CN102703983A (en) | 2012-06-15 | 2012-06-15 | Method and device for compressing free space in cadmium zinc telluride crystal growing crucible through double sealing sleeves |
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| CN2012101969259A CN102703983A (en) | 2012-06-15 | 2012-06-15 | Method and device for compressing free space in cadmium zinc telluride crystal growing crucible through double sealing sleeves |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911666A (en) * | 2013-01-08 | 2014-07-09 | 广东先导稀材股份有限公司 | Tellurium zinc cadmium polycrystal synthesis tool and tellurium zinc cadmium polycrystal synthesis method |
| CN106707326A (en) * | 2016-12-21 | 2017-05-24 | 兰州空间技术物理研究所 | Space X ray, electron and proton integrated detection probe |
| CN110366612A (en) * | 2018-02-09 | 2019-10-22 | Ｊｘ金属株式会社 | Compound semiconductor and its manufacturing method |
| CN113174626A (en) * | 2021-04-25 | 2021-07-27 | 合肥庞碲新材料科技有限公司 | Method and device for growing tellurium-zinc-cadmium single crystal |
| CN114481327A (en) * | 2020-10-26 | 2022-05-13 | 昆明物理研究所 | Method and device for synthesizing cadmium zinc telluride crystal by PBN crucible |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102230213A (en) * | 2011-06-08 | 2011-11-02 | 上海大学 | Method for growing tellurium-zinc-cadmium crystals by using tellurium solvent solution method |
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2012
- 2012-06-15 CN CN2012101969259A patent/CN102703983A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102230213A (en) * | 2011-06-08 | 2011-11-02 | 上海大学 | Method for growing tellurium-zinc-cadmium crystals by using tellurium solvent solution method |
Non-Patent Citations (1)
| Title |
|---|
| 郁芳: "CdZnTe的晶体生长、器件设计的模拟以及vfBGA封装内部芯片断裂的研究", 《上海大学硕士论文》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911666A (en) * | 2013-01-08 | 2014-07-09 | 广东先导稀材股份有限公司 | Tellurium zinc cadmium polycrystal synthesis tool and tellurium zinc cadmium polycrystal synthesis method |
| CN106707326A (en) * | 2016-12-21 | 2017-05-24 | 兰州空间技术物理研究所 | Space X ray, electron and proton integrated detection probe |
| CN110366612A (en) * | 2018-02-09 | 2019-10-22 | Ｊｘ金属株式会社 | Compound semiconductor and its manufacturing method |
| CN114481327A (en) * | 2020-10-26 | 2022-05-13 | 昆明物理研究所 | Method and device for synthesizing cadmium zinc telluride crystal by PBN crucible |
| CN114481327B (en) * | 2020-10-26 | 2023-11-21 | 昆明物理研究所 | Method and device for synthesizing tellurium-zinc-cadmium crystal by adopting PBN crucible |
| CN113174626A (en) * | 2021-04-25 | 2021-07-27 | 合肥庞碲新材料科技有限公司 | Method and device for growing tellurium-zinc-cadmium single crystal |
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Application publication date: 20121003 |