WO2012152773A1 - Entrée de matière première permettant de fabriquer des cristaux d'oxyde à partir d'une charge fondue et son procédé de production - Google Patents

Entrée de matière première permettant de fabriquer des cristaux d'oxyde à partir d'une charge fondue et son procédé de production Download PDF

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Publication number
WO2012152773A1
WO2012152773A1 PCT/EP2012/058405 EP2012058405W WO2012152773A1 WO 2012152773 A1 WO2012152773 A1 WO 2012152773A1 EP 2012058405 W EP2012058405 W EP 2012058405W WO 2012152773 A1 WO2012152773 A1 WO 2012152773A1
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Prior art keywords
melting
container
raw material
melted
material input
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PCT/EP2012/058405
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English (en)
Inventor
Andrej MARKIEWICZ
Anatoly Shkulkov
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Polycor Sp. z o.o.
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Publication of WO2012152773A1 publication Critical patent/WO2012152773A1/fr

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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
    • 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
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • 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
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets

Definitions

  • the invention relates to a raw material input for manufacturing oxide crystals from melted load and a method of its production.
  • the invention can be applied in the oxide crystals production technology, especially in industrial technology for production of sapphire single crystals.
  • the oxide single crystals play an important role in today's technology, e.g. in optical devices, lasers or microelectronic devices.
  • the crystals of sapphire are somewhat special among contemporary crystals, first of all they are used in microelectronics for production of light-emitting diodes (LEDs).
  • crushed crystals which form the raw material input must have been previously created using another technique of crystal production.
  • sapphire crystals the crushed sapphire crystals are used that had been previously obtained using the Verneuil process.
  • the raw material input in the form of crushed crystals is placed within a container, melted and a new crystal growth is evoked on a crystallization seed.
  • the raw material input is known for the production process of lithium niobate single crystals from the melted load using the Czochralski process [2].
  • the raw material input is made of a piece of lithium niobate, synthesised to the polycrystalline form. This piece is placed within a container to get melted and conduct the crystal growth process on a crystallization seed.
  • the density of the synthesized input lies between 50 and 70% of a theoretical density of crystals.
  • Article [3] describes another known process of production of the lithium niobate being used as the raw material input.
  • the mixture of components having been previously prepared in fixed proportion, namely: oxides and/or carbonates of lithium and niobium, undergoes for 2-3 hours the phases of pressing and annealing at the temperature of 1050°C up to 1100°C.
  • the crystalline phases of lithium niobate are created out of the initial components and the raw material input is formed in the shape of a polycrysta l li ne block.
  • the a mount of the crysta l line phase of lithi u m niobate i n t he polycrystalline block is not less than 99.5%.
  • the drawback of production of the raw material input here is that the process is based on crystalline structure synthesis in the solid state with the methodology used in the ceramic technology. This approach causes the contamination of the raw material input during the lengthy phases of mixing, pressing and annealing. In this way the quality of the raw material input is low, which in turn results in the low quality of the crystals, originated by the contamination.
  • Publication [5] related to the known technological solution, describes the production of the raw material input by induction melting of the initial components in a cold melting- pot, forming a melted polycrystalline block and crushing this block into small bits.
  • the induction melting in a cold melting-pot is performed at the temperature exceeding the crystal melting point, which gives the possibility of leading the synthesis process in the liquid phase of the crystalline structure of a block and ensures 100% content of the crystalline phase.
  • the disadvantage of this production process of the raw material input is that an additional stage is necessary, introduced after the synthesis of the polycrystalline block, namely crushing the block into small bits before its introduction to a container that the crystal will be grown in.
  • the raw material input is contaminated and this lowers the quality of the crystals being grown.
  • the melting products can be contaminated with the material of the melting-pot.
  • the cold melting-pot is made of copper pipes with water cooling, hence the contamination with copper can take place.
  • the purpose of this invention is to raise the quality of oxide crystals and ensure the repeatability of the quality parameters of the crystals grown in the industrial production conditions, which eventually leads to lowering their price.
  • this purpose is reached, because the raw material input for manufacturing oxide crystals on a crystallization seed from melted load in a container is initially subject to synthesis from components to the form of a polycrystalline block, wherein said raw material input has the form of a melted polycrystalline block with the dimensions corresponding to the characteristic dimensions of the container and has the volume density not lower than 75% of the theoretical density of said oxide crystal and has the mass not lower than 75% of the ful l conta iner load (ie. not lower tha n .75% of mass of the raw material input going into the container).
  • the invention covers also a method of production of such a raw material input, according to which liquid phase synthesis of the initial components by induction melting in a cold melting-pot to form a melted polycrystalline block is performed, while simultaneously (in one and the same technological operation) forming the polycrystalline block having the dimensions corresponding to the characteristic dimensions of the container.
  • said liquid phase synthesis process is performed while shifting the melting zone of the initial components upwards in relation to the cold melting-pot, wherein a cold melting-pot is used having a full bottom and having the dimensions of the transversal cross- section corresponding to the characteristic dimensions of the transversal cross-section of the container.
  • said liquid phase synthesis process is performed in vacuum.
  • said oxide crystal is sapphire or yttrium-aluminium garnet.
  • the raw material input must be synthesised beforehand from the initial components of the defined composition and desired chemical purity using the process of induction melting in a cold melting-pot in a form of polycrystalline shape.
  • the polycrystalline block is formed with the dimensions corresponding to the dimensions of the container.
  • corresponding dimensions or “similarity of dimensions” of the polycrystalline shape (block) it is understood that the block can be easily put into the container, having at the same time a similar shape.
  • the cold melting-pot must be prepared in such a way that its transversal cross-section should have similar shape and dimensions to the cross- section of the container.
  • the ratio of density of melted mass to the theoretical crystal density usually lies within the range of 0.7 to 0.75.
  • the volume density of the polycrystalline shape should not be lower than 75% of the theoretical crystal density. In such a way the effectiveness of crystal growing devices reaches its maximum, this leading to lowe ri ng of the price of crysta ls.
  • Usi ng the raw materia l i n puts with homoge neous composition as well as eliminating of additional steps related to their preparation prevents them from getting contaminated.
  • the raw material input should consist of at least 75% of the polycrystalline shape, and the remaining part can be made of remnants from treatment of the same crystals re-directed back to the production phase or other raw materials.
  • induction melting in a cold melting-pot allows for performing at the same time the liquid phase synthesis, which enables creation of monophase polycrystalline structure of the raw material input, as well as enables formation of the raw material input having dimensions corresponding to those of the container.
  • the induction melting in a cold melting-pot is considered to be a pure process of synthesis of crystalline materials, however during melting the products of the synthesis are contaminated with the material of the melting-pot, wh ich usua l ly is co p pe r. The contamination takes place as a result of high-temperature chemical reactions between active dopants being part of initial components, for example compounds of chlorine, sulphur or nitrogen, absorbed by the initial components during their own process of production in the chemical industry.
  • the layer of copper compounds gets partially melted and copper enters the melted load, thus conta minati ng it. It is possi ble to mi nimise or eli minate the tra nsfer of the melting-pot materia l into the melted load when the melti ng zone is consta ntly moved upwards in relation to the melting-pot. I n this case the copper compounds as well as said active dopants coming from original components of the raw material input, form a thin layer over the melting-pot walls and do not affect the heat transfer conditions of the melting-pot, which in turn limits or eliminates the transfer of melting-pot material to the melted load.
  • the core effect of the invention lies in the fact that it is ensured that the raw material input used for growing of crystals is prepared in the optimal way.
  • the raw material input in the process of liquid phase synthesis is transformed into a homogeneous form of polycrystalline block, with the dimensions corresponding to the dimensions of the container, as well as with the minimum amount of contaminants introduced during the process of synthesis and shaping.
  • Such a preparation of the raw material guarantees production of homogeneous high-quality crystals in the large-scale industrial processing.
  • the invention is presented in a photograph in the attached drawing.
  • the photograph shows polycrystalline blocks of corundum (aluminium oxide) with the diameter of 148 mm, intended to be used as the raw material input within a tungsten container having the diameter of 200 mm in the Kyropoulos-Musatov process for growing sapphire crystals.
  • Example 1 Production of the raw material input for the Kyropoulos-Musatov process of growing the crystals of sapphire on a crystallization seed from melted load in a container.
  • the crystal growing device is equipped with a tungsten container having the diameter of 200 mm.
  • the inner chamber of the container is in the shape of truncated cone. Its smaller diameter at the bottom of the container is 150 mm, its greater diameter is 155 mm, the working depth is 220 mm and the maximum depth is 240 mm.
  • the characteristic cross- section shape of the container circle.
  • the optimum raw material mass lies between 12 and 12.2 kg.
  • the raw material input is synthesised from the initial component, being the aluminium oxide powder of high chemical purity, freely available in the market, branded SPA-AC and produced by Sasol North America INC Ceralox Division with the ⁇ and a phases present.
  • the synthesis is done through induction melting in a cold melting-pot.
  • the full- bottom melting-pot is used, made of cooled copper tubes welded to the bottom, which in turn is sim ultaneously used as a cooling water separator.
  • the melting zone of the cold melting-pot is com pa ra ble to the cha racteristic di mensions of the conta i ne r, i .e . the diameter of its circular cross-section is 150 mm.
  • the working depth of the cold melting-pot is 300 mm.
  • the synthesis of the raw material input in the form of polycrystalline shape is done in the open air environment in the following way.
  • a portion of the oxide powder with the mass of 12.5 kg is taken.
  • a part of this portion placed in the cold melting-pot for initial heating, for example though creating an exothermic reaction of oxidising the shavings of metallic aluminium of high chemical purity.
  • the initial melted mass load is formed, which is subsequently heated in the electromagnetic field of the inductor and occupies the whole cross-section of the cold melting-pot.
  • the temperature of the melted mass lies within the range of 2100-2150°C.
  • the induction melting of the aluminium oxide is performed by introduction of the aluminium oxide powder to the melting zone of the cold melting-pot.
  • the melting zone is shifted upwards in relation to the melting-pot.
  • the crystallization process of the melted mass as the corundum phase occurs and the polycrystalline block is formed, with the transversal cross-section corresponding to the cross-section of the cold melting-pot. I n this way the synthesis of the polycrystalline block is done and the block itself is formed into the shape of the container. After the whole portion of the aluminium oxide powder has been added, the induction melting process is finished and the melted mass gets crystallized.
  • a melted polycrystalline corundum block is produced, with the mass of 12.1 kg, cylindrical cross-section having the diameter of 148 mm and the height of 235 mm.
  • the volume density of the polycrystalline corundum block is 3.0 g/cm 3 , which is 76% of the theoretical density of the sapphire crystal.
  • This polycrystalline block can be easily inserted into the container, ensuring at the same time the optimum filling of the container in a single operation.
  • the attached photograph presents two identical polycrystalline corundum blocks with the diameter of 148 mm produced by the process described above. After the polycrystalline block has been introduced into the container and melted, the melted mass of the aluminium oxide is on the optimal level.
  • the sapphire crystals grown of such a synthesised polycrystalline block are of high quality. They are transparent to the ultraviolet radiation, which qualifies them as crystals having minimum amount of contaminants.
  • Table 1 presents the results of the analysis of chemical composition and the amount of contaminants in source aluminium oxide powder as well as in two polycrystalline blocks of corundum produced - through the induction melting synthesis in a cold melting-pot having a full bottom - in two production cycles of the raw material input. As it can be seen, the raw material input has not been contaminated with copper from the cold melting-pot.
  • Example 2 Synthesis of the raw material input for the Kyropoulos-Musatov process of growing the single crystal of sapphire in a device having a tungsten container with the diameter of 300 mm.
  • the characteristic shape of the transversal cross-section of the container is the same as in the Example 1: cicular shape, diameter at the bottom: 260 mm, working depth: 260-280 mm.
  • Optimum weight of the raw material input lies within the range of 60 to 66 kg.
  • the synthesis is performed using the induction melting process in a cold melting-pot.
  • the melting-pot is of the same type as described in the Example 1, however the dimensions of the melting zone of the cold melting-pot correspond to the characteristic dimensions of the container, i.e. the diameter of this zone is 254 mm and its depth 450 mm.
  • the synthesis of the polycrystalline block is performed in vacuum.
  • a portion of aluminium oxide powder, identical as in the Example 1, and having the same composition as in the Example 1, having the mass of 10 kg, is introduced into the cold melting-pot located in the vacuum working chamber, for performing the initial heating process.
  • the necessary amount of the aluminium oxide is introduced into a tray, linked with the working chamber through a feeder.
  • the air is pumped out from the working chamber and the tray until the residual pressure of lxl0 "4 tor is achieved.
  • the induction heating is turned on and the initial melting of the aluminium oxide powder is performed by a known process.
  • the initial melted mass load is formed, which is then heated in the electromagnetic field of the inductor and which occupies the entire transversal cross-section of the cold melting-pot.
  • the induction melting of the oxide takes place by dosing the aluminium powder from the tray into the melting zone of the cold melting-pot. As the melting proceeds, the melting zone is shifted upwards in relation to the melting-pot. Crystallization of the melted mass occurs and q polycrystalline corundum block is formed, having the dimensions similar to the dimensions of the container, as in the Example 1.
  • the working chamber is opened and the block is taken out.
  • the block produced has the same dimensions as the container.
  • the mass of the synthesised block is in the range of 58-60 kg.
  • the volume density of the block is 95% to 97% of the theoretical density of the sapphire crystal.
  • the crystals grown as described in Example 2 have lower density of crystalline lattice defects, lower amount of contaminants and ensure higher productivity of the ready-made product that can be used for further processing.
  • Example 3 Synthesis of the raw material input for the horizontally-directed crystallization process (Bagdasarov process) of growing the yttrium-aluminium garnet crystals.
  • the device is equipped with a container of the "boat" shape, having the rectangular shape, having the dimensions of 40 mm of height and 90 mm of width.
  • the length of the container is 250 mm.
  • the crystallization seed is placed in the apex of the triangular part.
  • the container is being moved in the horizontal direction with respect to a heater, made in the form of a rectangular tungsten coil surrounding the container and connected to the source of electrical current.
  • the whole heat source is placed in a vacuum chamber.
  • the synthesis of the raw material input is done by a process of induction melting in a cold melting-pot of the stoichiometric mixture of initial components: aluminium oxide powder and yttrium oxide powder.
  • the cold melting-pot is produced with the full bottom and its transversal cross-section has di mensions com para ble to the dimensions of the container's cross-section, i.e. in this case it is a rectangle with the dimensions of 40 mm x 90 m m.
  • I nitia l heating of the stoichiometric mixture is conducted i n course of isotherma l reaction to oxidation of meta llic yttrium .
  • I n order to com pensate for the cha nge in the composition of the initial melted mass load a pre-calculated amount of aluminium oxide is introduced into the mass load.
  • the technological process of synthesis of the raw material input is performed as described in Example 1, however at the melted mass temperature of 2150-2200°C.
  • a rectangular polycrystalline block is formed, with the di mensions correspondi ng to the characteristic dimensions of the container.
  • the synthesis is terminated when the length of the block is equal to 180 m m.
  • the structure of the synthesised polycrystalline block is a monophase structure of aluminium-yttrium garnet. Its volume density is about 90% of the theoretical crystal density.
  • the polycrystalline block has dimensions corresponding to the di mensions of the conta i ner (the "boat) which a l lows to i ntrod uce the synthesized polycrystalline block into the container without any additiona l treatment. If needed, the tria ngu la r pa rt of the "boat” ca n be loaded with waste coming from treatment of the previously grown crystals, in order to ensure the optimal mass of the raw material input. The high quality of the raw input guarantees obtaining of high-quality single crystals.
  • Avtorskoe svidetelstvo 1329208 (SSSR). Sposob vyrashchivaniya tugoplavkikh monokristalov. MPK S W 17/00.

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  • 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

La présente invention concerne une entrée de matière première permettant de fabriquer des cristaux d'oxyde sur un germe de cristallisation à partir d'une charge fondue dans un contenant, que l'on a synthétisé à l'origine à partir de constituants pour obtenir la forme d'un bloc polycristallin. L'invention est caractérisée en ce que ladite entrée de matière première présente la forme d'un bloc polycristallin fondu dont les dimensions correspondent aux dimensions caractéristiques du contenant et présente une densité volumique non inférieure à 75 % de la densité théorique dudit cristal d'oxyde et dont la masse n'est pas inférieure à 75 % de la charge totale du contenant. Cette invention concerne également un procédé de production de l'entrée de matière première permettant de fabriquer des cristaux d'oxyde sur un germe de cristallisation à partir d'une charge fondue dans un contenant, comprenant la synthèse en phase liquide des constituants initiaux par fusion par induction dans un creuset froid, pour former un bloc polycristallin fondu. L'invention est caractérisée en ce que ledit procédé de synthèse en phase liquide est effectué en même temps que la formation du bloc polycristallin dont les dimensions correspondent aux dimensions caractéristiques du contenant.
PCT/EP2012/058405 2011-05-10 2012-05-07 Entrée de matière première permettant de fabriquer des cristaux d'oxyde à partir d'une charge fondue et son procédé de production WO2012152773A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PLP-394818 2011-05-10
PL394818A PL224041B1 (pl) 2011-05-10 2011-05-10 Wsad surowcowy do wytwarzania kryształu tlenkowego będącego szafirem na zarodku krystalizacji z masy stopionej i sposób otrzymywania takiego wsadu surowcowego

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT524441A4 (de) * 2020-12-29 2022-06-15 Fametec Gmbh Formkörperteil zur Herstellung eines Formkörpers

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4007220A1 (de) * 1990-02-20 1991-08-22 Norddeutsche Schleifmittel Ind Stoff, enthaltend kristallines a1(pfeil abwaerts)2(pfeil abwaerts)o(pfeil abwaerts)3(pfeil abwaerts), sowie verwendung und herstellungsverfahren
US20070031610A1 (en) * 2005-08-02 2007-02-08 Radion Mogilevsky Method for purifying and producing dense blocks
US7381266B1 (en) 2006-12-27 2008-06-03 Yu-Feng Chang Sapphire crystal growth method
EP2070873A1 (fr) * 2006-09-19 2009-06-17 Sumitomo Chemical Company, Limited Poudre d'alumine alpha
CN101913636A (zh) * 2010-08-20 2010-12-15 李振亚 用于蓝宝石单晶的高纯高密氧化铝块体原料的生产方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4007220A1 (de) * 1990-02-20 1991-08-22 Norddeutsche Schleifmittel Ind Stoff, enthaltend kristallines a1(pfeil abwaerts)2(pfeil abwaerts)o(pfeil abwaerts)3(pfeil abwaerts), sowie verwendung und herstellungsverfahren
US20070031610A1 (en) * 2005-08-02 2007-02-08 Radion Mogilevsky Method for purifying and producing dense blocks
EP2070873A1 (fr) * 2006-09-19 2009-06-17 Sumitomo Chemical Company, Limited Poudre d'alumine alpha
US7381266B1 (en) 2006-12-27 2008-06-03 Yu-Feng Chang Sapphire crystal growth method
CN101913636A (zh) * 2010-08-20 2010-12-15 李振亚 用于蓝宝石单晶的高纯高密氧化铝块体原料的生产方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
D.VIVIEN; A.M.LEJUS: "Observation de l'effet laser continu dans l'aluminate La0,9Nd0,1MgAl11O19 monocristallin (LNA) elabore par la methode Crochralski", C.R. ACAD. SC. PARIS. T., vol. 298, 1984, pages 195 - 198, XP000712589
FEDULOV A.S.; SHAPORO Z.I.; LODYZHINSKIJ I. B.: "Primenenie metoda Chokhralskogo dla vyrashchivaniya monokristallov LiNb03, LiTa03, NaNb03. AN SSSR", KRISTALLOGRAFIYA, vol. 10, no. 2, 1965, pages 268 - 270, XP008153239
OU YONGZONG: "GROWTH OF HIGH QUALITY LARGE Nd:YAG CRYSTALS TEMPERATURE GRADIENT TECHNIQUE (TGT)", JOURNAL OF CRYSTAL GROWTH, ELSEVIER, AMSTERDAM, NL, vol. 78, no. 1, 1 October 1986 (1986-10-01), pages 31 - 35, XP001302285, ISSN: 0022-0248 *
PARFITT H.T.; ROBETSON D.S.: "Domain structures in lithium niobate crystals", BRITISH J. APPLIED PHYSICS, vol. 18, 1967, pages 1709 - 1713, XP008153241, DOI: doi:10.1088/0508-3443/18/12/305

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT524441A4 (de) * 2020-12-29 2022-06-15 Fametec Gmbh Formkörperteil zur Herstellung eines Formkörpers
AT524441B1 (de) * 2020-12-29 2022-06-15 Fametec Gmbh Formkörperteil zur Herstellung eines Formkörpers

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PL394818A1 (pl) 2012-11-19

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