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1

Ceramiczne nadprzewodniki wysokotemperaturowe – otrzymywanie proszków YBa2Cu3O7-x metodami syntezy w fazie stałej i w plazmie

Szterner P., Pęczkowski P., Jaegermann Z.

Prace Instytutu Ceramiki i Materiałów Budowlanych

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2017

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R. 10, nr 29

48--60

PL

Artykuł jest pracą przeglądową, stanowiąc kontynuację cyklu publikacji dotyczących ceramicznych nadprzewodników wysokotemperaturowych ze zwróceniem szczególnej uwagi na nadprzewodnik z rodziny miedzianów – YBa2Cu3O7-x. Związek YBa2Cu3O7-x nazywany jest też YBCO lub Y-123 ze względu na skład stechiometryczny. Należy on do najważniejszych materiałów ceramicznych o właściwościach nadprzewodzących. W artykule przedstawiono różne techniki otrzymania YBa2Cu3O7-x. Szczególny nacisk położono na zobrazowanie metod syntezy w fazie stałej i w plazmie oraz na scharakteryzowanie ich zalet i wad.

EN

This paper is a review and continuation series of articles on ceramic high-temperature superconductors with particular attention to the superconductor family of cuprates – YBa2Cu3O7-x. The YBa2Cu3O7-x compound, called also YBCO or Y-123 on account of stoichiometric composition, is one of the most important superconducting materials. In this paper, different methods useful for obtain YBa2Cu3O7-x powder have been presented. Particular emphasis was placed on method of synthesis in solid state and plasma and characterize their merits and flaws.

2

Ceramiczne nadprzewodniki wysokotemperaturowe – otrzymywanie YBa2Cu3O7-x metodami prażenia

Szterner P., Pęczkowski P., Jaegermann Z.

Prace Instytutu Ceramiki i Materiałów Budowlanych

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2017

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R. 10, nr 28

62--75

PL

Artykuł jest pracą przeglądową, stanowi kontynuację cyklu publikacji dotyczących ceramicznych nadprzewodników wysokotemperaturowych, ze zwróceniem szczególnej uwagi na nadprzewodnik z rodziny miedzianów YBa2Cu3O7-x (nazywany też YBCO lub Y-123). Należy on do najważniejszych ceramicznych materiałów nadprzewodzących. W artykule przedstawiono podział na różne techniki otrzymania YBa2Cu3O7-x, a bardziej szczegółowo opisano otrzymywanie YBCO konwencjonalną metodą prażenia.

EN

This review paper continues a series of articles on ceramic high-temperature superconductors, with particular attention to the superconductor family of cuprates YBa2Cu3O7-x. (called also YBCO or Y-123). It belongs to most important superconducting materials. In this paper, the division into different methods for obtaining YBCO ceramics have been presented. Conventional ceramic process for obtaining of YBCO, namely calcination, has been described in more detail.

3

Synthesis and characterization of luminescent Er, Nd and Dy doped Ba3BP3O12

Çelik Gül G., Kurtuluş F.

Archives of Materials Science and Engineering

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2017

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Vol. 83, nr 2

68--73

EN

Purpose: Purpose of this study, our aim is high temperature based on synthesis method of barium borophosphate and doping with lanthanide type metals such as Er, Nd and Dy into the structure by solid state reaction. Design/methodology/approach: The starting materials rare earth oxides, barium carbonate, boric acid and ammonium dihydrogen phosphate as analytically grade weighed 0.01:3:1:3 molar ratio and homogenized in an agate mortar. The mixture placed into a porcelain crucible to heat in high temperature oven step by step. First, mixtures waited at 400°C for 2 hours for calcination process, subsequently heated 900°C with step rate 10°C/m for 8 hours, and finally cooled down to room temperature with step rate 10°C/m. After many grindings final product get ready for characterization. X-ray powder diffraction (XRD) analysis was performed using PANanalytical X’Pert PRO Diffractometer (XRD) with Cu Kα (1.5406 Å, 45 kV and 30 mA) radiation. Fourier transform infrared spectroscopy (FTIR) was taken on a Perkin Elmer Spectrum 100 FTIR Spectrometer from 4000 to 650 cm-1. Scanning electron microscopy was achieved in SEM JEOL 6390-LV. Luminescence properties were performed by Andor Solis Sr 500i spectrophotometer. Conventional solid state syntheses were done in Protherm furnace. Findings: The XRD patterns of the samples show that 0.01 wt.% Er:Ba3BP3O12, 0.01 wt.% Nd:Ba3BP3O12 and 0.01 wt.% Dy:Ba3BP3O12 compounds were obtained as pure phase. When the pattern of the samples is compared to the International Centre for Diffraction Data (ICDD) cards, it gets along with Ba3BP3O12 crystallized in tetragonal system In the XRD pattern of the samples, there is no reflection born of rare earth metal oxides. Research limitations/implications: The synthesis method has some disadvantages such as low homogeneity, non-uniform product etc. We tried to minimize these negative aspects in our research and succeeded. Practical implications: Implications Luminescent Er:Ba3BP3O12, Nd:Ba3BP3O12 and Dy:Ba3BP3O12 compounds were synthesized by conventional solid state method completely different from literature for the first time. The characterization was mainly based on powder X-ray diffraction pattern. Also, luminescence and morphological properties were determined. Originality/value: Value of the paper is first time conventional synthesis of Er, Nd and Dy doped Ba3BP3O12 compounds, calculation of unit cell parameters, and investigation of morphological and luminescent properties.

4

Optimization of Selected Parameters of Refractory Solid Solution Formation With Essential Storage and Transport Properties

Śnieżek E., Szczerba J., Prorok R., Jastrzębska I.

Logistyka

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2014

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nr 4

4981--4988, CD6

EN

The work presents (Ca,Sr)ZrO3 solid solution formation which isresistant to hydration and thus having important properties to facilitate storage and transport.The paperraises the issue of effective selection of synthesis parameters. In this case analysis of phase diagrams, also literature data analysis, provide essential information about predicted properties and preparation conditions of matter. On this basis, sampleswere prepared by a solid state reaction. (Ca,Sr)ZrO3 solid solution were obtained during two-step heat treatment at 1200 and 1400°C. X-ray diffraction, Scanning Electron Microscopy and mercury poro-simetry were used to check and examine obtained samples.

PL

Artykuł opisuje proces tworzenia się roztworu stałego, (Ca,Sr)ZrO3 odpornego na hydratację a tym samym posiadającego istotne właściwości ułatwiające magazynowanie i transport. Porusza on zagadnie-nie związane z efektywnym doborem parametrów procesu na bazie analizy diagramów fazowych i danych literaturowych, które pozwalają w pewnym stopniu przewidzieć zastosowanie niezbędnych warunków i potencjalne właściwości otrzymanych substancji. Bazując na tych danych wybrano proces syntezy przebiegającej w fazie stałej. (Ca,Sr)ZrO3otrzymano w wyniku dwustopniowego wypalania w 1200 i 1400°C. Próbki scharakteryzowano metodą XRD, SEM/EDS i porozymetrii rtęciowej.

5

Synteza i właściwości luminescencyjne Sr2CeO4

Korczyc B., Lipińska L., Diduszko R., Surma B.

Materiały Elektroniczne

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2011

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T. 39, nr 1

36-39

PL

Sr2CeO4 stanowi atrakcyjny materiał ze względu na praktyczną możliwość wykorzystania go w przemyśle np. w konstrukcji wyświetlaczy z emisją polową. Zsyntetyzowano luminofor za pomocą dwóch niezależnych metod. W każdej z nich zostały wykorzystane inne rodzaje substratów. Zbadano skład fazowy produktów za pomocą analizy rentgenowskiej XRD, mikrostrukturę za pomocą skaningowej mikroskopii elektronowej SEM oraz wykonano pomiary luminescencji.

EN

From an industrial perspective, Sr2CeO4 is a particularly promising material because of the possibility of its practical application, for example to the construction of field emission displays. In this work, phosphor was synthesized by two independent techniques, namely a solid state method and a sol-gel method using different starting chemicals. The phase composition was examined by an X-ray diffraction method (XRD), whereas microstructure by scanning electron microscopy (SEM). In the end, the luminescence spectra were recorded.

6

Narzędzia chemii kombinatorycznej. Cz. 4. Synteza asymetryczna na fazie stałej

Łaźny R., Nodzewska A., Żabicka B.

Wiadomości Chemiczne

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2006

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[Z] 60, 3-4

191-255

EN

Solid Phase Asymmetric Synthesis (SPOS) is a recently introduced term embracing all methods of asymmetric synthesis involving use of solid supported substrates and reagents. This review presents basic definitions of asymmetric synthesis and currently used concepts for enatioselective and diastereoselective transformations involving supported synthesis. The concepts of chiral auxiliary, chiral catalyst and chiral reagent are illustrated with selected but fairly comprehensive overview of methods published till January 2005. In particular use of chiral auxiliaries such as oxazolidine derivatives, amines, hydrazines, sulfoxides, sulfinyl amides, sulfoxy imines, carbohydrates and alcohols is covered. Applications of immobilized chiral catalysts to synthesis of carbon-carbon bonds, carbon-hydrogen bonds, carbon--heteroatom bonds and in phase-transfer catalysis is presented with selected reactions due to huge volume of literature in this field. Moreover applications of chiral catalysts and chiral reagents in reactions of immobilized substrates and use of chiral immobilized reagents is also reviewed. The literature review shows that the most popular methods of supported asymmetric synthesis are the alkylation of enolates, aldol reactions, Grignard reactions, cycloadditions, reduetion of ketones, epoxida-tions, olefin dihydroxylation, and phase-transfer catalyzed reactions. There are numerous applications of immobilized chiral catalysts and a substantial number of applications of immobilized chiral auxiliaries. On the other hand there are only scarce reports of applications of chiral reagents and chiral catalysts to the reactions of achiral immobilized substrates.

7

Synteza w fazie stałej biologicznie czynnego analogu hormonu GH-RH potencjalnego leku w schorzeniach związanych z niedoborem hormonu wzrostu

Bańkowski K.

Przemysł Chemiczny

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2006

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T. 85, nr 5

330-332

PL

Przedstawiono syntezę w fazie stałej 29-aminokwasowego peptydu A, analogu hormonu uwalniającego hormon wzrostu GH-RH. Właściwości biologiczne tego peptydu wskazują, że może on stać się cennym lekiem hormonalnym w leczeniu wszelkich schorzeń związanych z niedoborem hormonu wzrostu, np. karłowatości u dzieci. Opracowano formę farmaceutyczną dla tej substancji.

EN

A 100–200-mesh methoxybenzhydrylamine resin was used as a solid carrier. The first amino acid was introduced on the resin, and all 28 amino acids of peptide A were subsequently coupled, by the carbodiimide method. The a a a a a -amino function was protected with BOC group, and the side chains were blocked with the following groups: Asp, cyclohexyl; Ser and Thr, benzyl; and Tyr 2-bromobenzyloxycarbonyl. Boc(Fmoc)Lys were added at positions 11, 12, 20, 21 and 29 to have at further steps the analog contg. hArg in these positions. Boc was removed with 55% TFA in dichloromethane, and Fmoc was removed with 50% piperidine in DMF. After Fmoc was removed from Lys, the substituted guanidine group was introduced by the reaction with N,N’- bis(tert-butyloxycarbonyl)-S-methylisothiourea in the presence of 4-(N,N N dimethylamino)pyridine. All Boc were removed from the fully protected peptidyl polymer by the reaction with trifluoroacetic acid. The remaining protecting groups left the peptide while it was cleaved from the resin with liq. HF. The HF was removed, the residue was washed with Et2O, and crude peptide was extd. with 50% AcOH and lyophilized. The acetate form was obtained on an ion-exchange resin and preparative HPLC gave 99.7% pure A. Polysulfonic filters were used during the preparation of the stable and reproducible pharmaceutical form of A, viz., an aq. lyophilizate (phosphate buffer) contg. 100 µg peptide A and mannitol per ampule. Peptide A was about a few score times as bioactive as the hGH-RH reference peptide, completely nontoxic in doses up to 120 ìg and resistant to enzymatic degradation, increased the level of hGH and the no. of somatotropic cells in animal pituitary glands, and affected no other pituitary hormones.

8

Narzędzia chemii kombinatorycznej. Cz 3. Reakcje w syntezie organicznej na fazie stałej

Łaźny R., Łapińska M., Sienkiewicz M.

Wiadomości Chemiczne

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2005

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[Z] 59, 11-12

881--952

EN

Solid Phase Organic Synthesis (SPOS) is a dynamically growing branch of organic synthesis encompusing methods for synthesis of both small molecules and oligomers on solid supports. Synthetically useful organic reactions of substrates immobilized on solid supports constitute a central part of the methodology of solid phase synthesis. This review article presents a representative and fairly comprehensive overview of reactions of supported substrates published till January 2005. The reactions are classified in synthetic terms into functional group interconvertions (FG1, according to type of functional group reacting and prepared) and C-C bond forming reactions (according to reaction type; usually name reaction). Fn particular preparations of halogens, alcohols, ethers, thiols, aldehydes, ketones, acids, esters, amides, phosphines, amines, poliamines, peptides, peptoids, oligonucleotides, and oligosaccharides is covered. Oxidation reactions of alcohols, aldehydes and ketones as well as reduction reactions of aldehydes, ketones, esters, acids, nitro and nitroso compounds are also presented. Only the selected reactions used for preparation of oligonucleotides, oligosaccharides, and polypeptides are covered due to the large volume of literaturę on this topie. The important C-C bond forming reactions such as Mannich, Michael, aldol, Heck, Suzuki, Stille, Sonogashira, Wittig, Horner-Wad-sworth-Emmons, metathesis, carbonyl compound alkylation and acylation reactions are illustrated with examples. Moreover the multicomponent reactions such as Ugi reaction, Hantzsch reaction and Baylis-Hillman reaction are also included in the review. The literature review shows a spectrum of synthetic organic reactions which can be performed on the immobilized substrates and suggests that in principle every reaction could be performed on solid phase. Howeverthe literature review indicates that reactions of polar organometallic reagents, radical reactions, and enantioselective reactions of achiral immobilized substrates are rather rarely used in SPOS.

9

Polimerowe kwasy nadtlenokarboksylowe i nadtlenosulfonowe - synteza, właściwości i kierunki zastosowania

Pińkowska H.

Prace Naukowe Instytutu Technologii Organicznej i Tworzyw Sztucznych Politechniki Wrocławskiej. Konferencje

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2001

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Vol. 50, nr 23

294-297

PL

Celem pracy była synteza metodami bezpośrednimi i/lub pośrednimi polimerycznych kwasów nadtlenokarboksylowych i nadtlenosulfonowych, określenie ich właściwości fizykochemicznych oraz wyznaczenie kierunków zastosowania. Do badań nad chemiczną transformacją grup karboksylowych i sulfonowych za pomocą H2 O2 i innych czynników utleniających w obecności kwasowych katalizatorów reakcji zostały wykorzystane dostępne w handlu kopolimery: 1. kwasu akrylowego i/lub metakrylowego i diwinylobenzenu, 2. styrenu i diwinylobenzenu, zawierające grupy sulfonowe. Do badań wybrano kopolimery pochodzące z firm Rohm&Haas, Bayer-Lewatit i Bio-Rad, różniące się zawartością grup funkcyjnych, odmiennym usieciowaniem matrycy polimerowej diwinylobenzenem oraz fizyczną strukturą ziaren (żelowe i makroporowate). Zbadano wpływ rodzaju matrycy kopolimerycznej i parametrów reakcji syntezy na uzyskane wyniki.

EN

Chemical modification - solid phase synthesis of peracid-type resins by oxidation of carboxylic and/or sulfonic acid-type ion exchangers with hydrogen peroxide aqueous solutions in sulfonic and sulfuric acid media has been studied. The starting materials were commercial cross-linked acrylic acid and/or polystyrene resins. Influence of composition of the resins and aci concentration of the media on the conversion of carboxylic to percarboxylic and/or sulfonic acid groups in the resins is discussed. Conditions for the oxidation, including the catalyst, reaction time, and effect of temperature on conversion were investigated.