CN106012013A - Method for growing lead iodide single crystals - Google Patents
Method for growing lead iodide single crystals Download PDFInfo
- Publication number
- CN106012013A CN106012013A CN201610523031.4A CN201610523031A CN106012013A CN 106012013 A CN106012013 A CN 106012013A CN 201610523031 A CN201610523031 A CN 201610523031A CN 106012013 A CN106012013 A CN 106012013A
- Authority
- CN
- China
- Prior art keywords
- lead iodide
- lead
- iodide
- liquid
- ingot casting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
-
- 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
- C30B29/12—Halides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the field of energy conservation and environment protection and particularly relates to a method for growing lead iodide single crystals. The lead iodide single crystals conform to the stoichiometric proportion. The method includes the steps that lead iodide seed crystals are placed, and lead iodide precast ingots are melted and crystallized, wherein the lead iodide seed crystals are placed on the lead iodide precast ingots and make contact with the lead iodide precast ingots, the atom molar ratio of lead to iodine in the lead iodide seed crystals and the lead iodide precast ingots is 1:1.95 to 1:2.05; during melting and crystallization, the lead iodide seed crystals are kept in a solid state, the lead iodide precast ingots are sequentially heated from top to bottom in the vertical direction and sequentially melted into liquid lead iodide from top to bottom, and liquid lead iodide is crystallized in the process; the temperature of liquid lead iodide ranges from 410 DEG C to 450 DEG C, and the temperature gradient on a crystallization interface between liquid lead iodide and the lead iodide seed crystals or the temperature gradient on a crystallization interface between liquid lead iodide and crystallized solid lead iodide ranges from 5 DEG C/cm to 30 DEG C/cm.
Description
Technical field
The present invention relates to iodine field, a kind of method growing lead Iodide single crystal.
Background technology
In prior art, the technique reclaimed for iodine is concentrated mainly on containing reclaiming iodine, phosphoric acid by wet process in iodine waste liquid
Production is reclaimed iodine；And the method reclaiming iodine in phosphoric acid by wet process mainly has two kinds: (1) adds in phosphoric acid by wet process
Enter certain oxidant, it may be possible to chlorine, potassium permanganate, potassium chlorate or hydrogen peroxide are strong with vanadic anhydride etc.
One or more mixing of oxidant, are oxidized to iodine molecule by iodine by the I-of free state, are subsequently adding four chlorinations
The extractants such as carbon, are sufficiently stirred for being extracted in organic facies iodine molecule, separate organic facies and acid solution phase, one
Evaporate carbon tetrachloride by decompression distillation mode under fixed temperature and pressure and obtain thick iodine；(2) add in phosphoric acid by wet process
Enter certain oxidant, it may be possible to chlorine, potassium permanganate, potassium chlorate or hydrogen peroxide are strong with vanadic anhydride etc.
One or more mixing of oxidant, are oxidized to iodine molecule by iodine by the I-of free state, blast air or nitrogen
Iodine molecule in phosphoric acid is blown out by gas, with dissolved with SO2 or Na2SO3 behind the iodine steam introducing absorption tower in air-flow
A kind of iodine solution absorb.Iodide solution flows out from the bottom of tower with finite concentration, adds chlorine, height in solution
One or more of the strong oxidizers such as potassium manganate, potassium chlorate or hydrogen peroxide and vanadic anhydride, stand and make list
Matter iodine separates out, and filters to obtain thick iodine.
Patent of invention content
Patent of the present invention provides a kind of method growing lead Iodide single crystal, to solve to carry in above-mentioned background technology
The problem of the not energy-conserving and environment-protective gone out.
Patent of the present invention is solved the technical problem that and is realized by the following technical solutions: the lead iodide seed of employing
Brilliant and the lead in the pre-ingot casting of lead iodide with iodine atomic molar ratio is 1: 1.95-1: 2.05, close to preferableization
Learn proportioning.Lead iodide seed crystal is placed on the top of the pre-ingot casting of lead iodide and is in contact with it, and when growth, keeps
The lead iodide seed crystal of top is solid-state, from the contact position of lead iodide seed crystal and the pre-ingot casting of lead iodide, to iodine
Change the pre-ingot casting of lead and carry out heating successively from top to bottom so that it is be molten into liquid lead iodide, and make lead iodide pre-
Ingot casting crystallizes the most successively from the contact position of lead iodide seed crystal.In crystal growing process, by
In lead iodide seed crystal above liquid lead iodide, eliminate the remaining space above liquid lead iodide, thus
Effectively prevent the iodine in liquid lead iodide to volatilize, and then prevent the decomposition of lead iodide, so that liquid iodophor
In change lead, lead remains 1 with the atomic molar ratio of iodine: 1.95-1: 2.05.Molten owing to present invention employs region again
The heating means of refining, the thermograde at crystalizing interface is 5-30 DEG C/cm, and this thermograde is to draw through experiment
The liquid lead iodide crystallization that can make will not separate out again the preferably thermograde of liquid lead, because this temperature simultaneously
Degree gradient is relatively big, makes to be at crystalizing interface the negligible amounts of the liquid lead iodide of supercooled state, liquid iodate
The probability that liquid lead core crash in lead is grown up reduces, thus does not has time enough to breed precipitation liquid lead,
Thus effectively prevent liquid lead iodide separation (when liquid lead iodide has liquid lead to separate out, liquid iodophor
Change lead and can be separated into liquid lead and the lead iodide of rich iodine) so that the lead Iodide single crystal that crystallization obtains keeps iodine
Changing the atomic molar ratio of the lead in the pre-ingot casting of lead and iodine, i.e. in crystal, the atomic molar of lead and iodine is 1 than also:
1.95-1∶2.05。
Accompanying drawing explanation
Fig. 1 is a kind of method structural representation growing lead Iodide single crystal of the present invention.
Detailed description of the invention
Embodiment:
The present embodiment includes: patent the most of the present invention is solved the technical problem that employing techniques below side
Case realizes: the invention belongs to a kind of method growing lead Iodide single crystal, and described placement lead iodide seed crystal is:
Described lead iodide seed crystal is placed on above the pre-ingot casting of described lead iodide, and ingot casting pre-with described lead iodide contacts,
Wherein, the lead in described lead iodide seed crystal and the pre-ingot casting of described lead iodide is 1: 1.95 with the atomic molar ratio of iodine
-1∶2.05；
Described it is molten into: keeping described lead iodide seed crystal is solid-state, and ingot casting pre-to described lead iodide is carried out vertically
Direction heating successively from top to bottom, makes the pre-ingot casting of described lead iodide be molten into liquid iodate the most successively
Lead；
Described crystallization is: when the pre-ingot casting of described lead iodide is molten into described liquid lead iodide the most successively,
Described liquid lead iodide is made to start to crystallize the most successively from the contact position of described lead iodide seed crystal；
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and also
Non-is the restriction to embodiments of the present invention.For those of ordinary skill in the field, above-mentioned
Can also make other changes in different forms on the basis of explanation.Here without also cannot be to all
Embodiment give exhaustive.All made within the spirit and principles in the present invention any amendment, equivalent replace
Change and improvement etc., within should be included in the protection domain of the claims in the present invention.
Claims (1)
1. the invention belongs to a kind of method growing lead Iodide single crystal, including placing lead iodide seed crystal and to iodine
Change fusing and the crystallization of the pre-ingot casting of lead,
Described placement lead iodide seed crystal is: be placed on by described lead iodide seed crystal above the pre-ingot casting of described lead iodide,
And ingot casting pre-with described lead iodide contacts, wherein, in described lead iodide seed crystal and the pre-ingot casting of described lead iodide
Lead is 1: 1.95-1: 2.05 with the atomic molar ratio of iodine；
Described it is molten into: keeping described lead iodide seed crystal is solid-state, and ingot casting pre-to described lead iodide is carried out vertically
Direction heating successively from top to bottom, makes the pre-ingot casting of described lead iodide be molten into liquid iodate the most successively
Lead；
Described crystallization is: when the pre-ingot casting of described lead iodide is molten into described liquid lead iodide the most successively,
Described liquid lead iodide is made to start to crystallize the most successively from the contact position of described lead iodide seed crystal；
Wherein, the temperature of described liquid lead iodide is made to be 410-450 DEG C, at the pre-ingot casting of described lead iodide from up to
Under be molten into described liquid lead iodide successively during, make described liquid lead iodide and described lead iodide seed crystal
Between crystalizing interface at or described liquid lead iodide and the lead iodide of solid-state crystallized between crystalizing interface
The thermograde at place is 5-30 DEG C/cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610523031.4A CN106012013A (en) | 2016-06-30 | 2016-06-30 | Method for growing lead iodide single crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610523031.4A CN106012013A (en) | 2016-06-30 | 2016-06-30 | Method for growing lead iodide single crystals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106012013A true CN106012013A (en) | 2016-10-12 |
Family
ID=57106554
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610523031.4A Pending CN106012013A (en) | 2016-06-30 | 2016-06-30 | Method for growing lead iodide single crystals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106012013A (en) |
-
2016
- 2016-06-30 CN CN201610523031.4A patent/CN106012013A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102933494B (en) | Utilize the method for cascade process purifying silicon | |
| US4200621A (en) | Sequential purification and crystal growth | |
| TWI429794B (en) | Method for purifying silicon | |
| CN101665253B (en) | Polysilicon purification method and crucible and purification device used for polysilicon purification | |
| Wu et al. | Boron removal from silicon using secondary refining techniques by metallurgical method | |
| CN106659975B (en) | The method that tritiated water is detached from light-water | |
| CN103180245A (en) | Fluorspar/iodide process for silicon purification | |
| Sun et al. | Preparation of high pure tellurium from raw tellurium containing Cu and Se by chemical method | |
| US20090098715A1 (en) | Process for manufacturing silicon wafers for solar cell | |
| TW200613265A (en) | Process for producing high-purity terephthalic acid | |
| CN106012013A (en) | Method for growing lead iodide single crystals | |
| JPS60137892A (en) | Quartz glass crucible | |
| CN101792143B (en) | Method for purifying silicon | |
| CN106283190A (en) | A kind of magnetic Solid-Phase Extraction material and preparation method thereof | |
| KR101180353B1 (en) | Refining method of Phosphorus and other impurities from MG-Si by acid leaching | |
| JP2009096709A (en) | Method and apparatus for purifying phosphoric acid by fractional crystallization | |
| TWI488818B (en) | Crucible and the method for purification of silicon using the same | |
| JP2007126342A (en) | Method of manufacturing silicon | |
| JP4392670B2 (en) | Manufacturing method of high purity silicon | |
| KR100882578B1 (en) | Czochralski apparatus for growing crystals and purification method of waste salts using the same | |
| CN101671027B (en) | Metallurgical silicon purification method and on-line slagging boron removal method | |
| JP4899034B2 (en) | Gallium raw material for compound semiconductor production | |
| US20140341795A1 (en) | Fluorspar/Iodide Process for Reduction, Purification, and Crystallization of Silicon | |
| CN101837980B (en) | Method for removing boron and phosphorus impurities in industrial silicon through sulphide | |
| JPH01156437A (en) | Method for refining indium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161012 |