TR201722696A2 - Synthesis of POSS-TX Nanophoto Initiator - Google Patents

Synthesis of POSS-TX Nanophoto Initiator Download PDF

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TR201722696A2
TR201722696A2 TR2017/22696A TR201722696A TR201722696A2 TR 201722696 A2 TR201722696 A2 TR 201722696A2 TR 2017/22696 A TR2017/22696 A TR 2017/22696A TR 201722696 A TR201722696 A TR 201722696A TR 201722696 A2 TR201722696 A2 TR 201722696A2
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poss
obtaining
synthesis
antibacterial
acrylic
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TR2017/22696A
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Öcal Nüket
Arsu Nergi̇s
Saadet Batibay Gönül
Tahi̇r Günkara Ömer
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Univ Yildiz Teknik
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Priority to TR2017/22696A priority Critical patent/TR201722696A2/en
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Priority to US16/957,622 priority patent/US11591418B2/en
Priority to PCT/TR2018/050924 priority patent/WO2019132848A1/en
Priority to DE112018006657.6T priority patent/DE112018006657B4/en

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Abstract

Buluş özellikle, Polioligosilseskioksan (POSS) yapısına sahip fotobaşlatıcıların sentezlenmesi ve bu fotobaşlatıcılar kullanılarak fotopolimerizasyonların gerçekleştirilmesi ve POSS yapısını içeren polimer matriksinde Ag nanoparçacıkların eş zamanlı ve in-situ sentezi sonucunda kırışık yüzeylerin elde edilmesi ile ilgilidir.In particular, the invention relates to the synthesis of photoinitiators having a polyoligosylsessoxoxane (POSS) structure and to perform photopolymerizations using these photoinitiators and to obtain wrinkled surfaces by the simultaneous and in situ synthesis of Ag nanoparticles in the polymer matrix comprising the POSS structure.

Description

TARIFNAME POSS-TX nanofotobaslaticinin sentezi ve POSS-TX yardimi ile yerinde fotokimyasal olarak Ag nanoparçacik sentezi ve kirisik yüzey olusumu Teknik Alan Bulus, esnek elektronik malzeme ve optik cihazlarda kullanilmak üzere, in-situ olarak kendiliginden düzenleme gerçeklesmis ve nanoboyutlu gümüs nanoparçaciklari içeren kirisik bir yüzey elde edilmesi ile ilgilidir. DESCRIPTION Synthesis of POSS-TX nanophotoinitiator and in situ photochemical analysis with the help of POSS-TX Ag nanoparticle synthesis and wrinkled surface formation Technical Area The invention is available in situ for use in flexible electronic materials and optical devices. self-regulating and wrinkle containing nanosized silver nanoparticles It's about obtaining a surface.

Bulus özellikle, Polioligosilseskioksan (POSS) yapisina sahip fotobaslaticilarin sentezlenmesi ve bu fotobaslaticilar kullanilarak fotopolimerizasyonlarin gerçeklestirilmesi ve POSS yapisini içeren polimer matriksinde Ag nanoparçaciklarin es zamanli ve in-situ sentezi sonucunda kirisik yüzeylerin elde edilmesi ile ilgilidir. The invention particularly focuses on the use of photoinitiators with Polyoligosylsesquioxane (POSS) structure. synthesis and realization of photopolymerizations using these photoinitiators and Simultaneous and in-situ synthesis of Ag nanoparticles in polymer matrix containing POSS structure As a result, it is related to the obtaining of creased surfaces.

Teknigin Bilinen Durumu Serbest radikal fotopolimerizasyon reaksiyonlari kaplamalarda, mikroelektronikte, fotorezist ve dolgu maddelerinde yaygin olarak kullanilmaktadir. Fotopolimerizasyon az enerji sarfiyati, düsük maliyet, uygun sicakliklarda ve az yer kaplamasi gibi üstün özelliklere sahip olmasindan dolayi diger sistemlere göre daha çok tercih edilmektedir. State of the Art Free radical photopolymerization reactions are used in coatings, microelectronics, photoresist and is widely used in fillers. Photopolymerization consumes less energy, It has superior features such as low cost, suitable temperatures and small footprint. It is preferred more than other systems because of its

Silseskioksan organosilikon bilesikler olup, RSIO3/2 empirik kimyasal formülüne sahiptir. R grubu alkil, alkenil, aril ya da arilen gruplarindan birisi olabilmektedir (1). Bahsedilen bu bilesikler katalizör olarak, pH ayarlamada görevli metaryeller olarak da kullanilmaktadir (2,3). Silsesquioxane are organosilicon compounds and have the empirical chemical formula RSIO3/2. R group can be one of alkyl, alkenyl, aryl or arylene groups (1). This is mentioned Compounds are also used as catalysts and as materials for pH adjustment (2,3).

Silseskioksanlar kafes seklindeki yapilar olup, çogunlukla küp, hekzagonal prizma, oktagonal prizma, dekagonal prizma, dodekagonal prizma formunda ya da bazen açik kafes formunda olabilmektedir. Silsesquioxanes are lattice-shaped structures, mostly cube, hexagonal prism, octagonal structures. prism, decagonal prism, dodecagonal prism or sometimes open lattice form can happen.

Silseskioksanlarin 3 boyutlu yapilari, yüksek simetrileri ve nanometre ölçeginde olmalari, nanobilesiklerin sentezinde önemli sentez yapisi olmasini saglamaktadir. Olasi fonksiyonel gruplarin 3 boyuttaki yönlenmesinin kontrolü bu nanometre ölçekli alisildik olmayan sentez yapilariyla saglanabilmektedir. Silika kafes, tipik organik moleküllerdeki gibi gerginligi ve termal kararliligi saglamaktadir. Silseskioksanlarin çesitli gruplarla türevlendirilmesi ile, fiziksel özellikleri degistirilebilmektedir. Böylelikle, Silseskioksanlarin tipik seramiklerden daha kolay islenebilmektedir. Organik ve anorganik gruplarla fonksiyonlandirilmis bu yapi sayesinde birçok nanometeryal malzeme yapilmaktadir. Bu malzemelerin özellikleri tipik polimer ve seramikten çok daha iyidir. Tüm bunlarin yani sira, silseskioksanlarin çesitli fonksiyonlandirma reaksiyonlari ile antimikrobiyal türevleri de sentezlenmektedir. Silsesquioxanes have 3-dimensional structures, high symmetry and nanometer scale. It provides an important synthesis structure in the synthesis of nanocomposites. Possible functional control of the 3-dimensional orientation of groups in this nanometer-scale non-usual synthesis can be provided with its structures. The silica lattice, like typical organic molecules, provides tension and It provides thermal stability. By derivatization of silsesquioxanes with various groups, physical properties can be changed. Thus, silsesquioxanes are more durable than typical ceramics. it is easy to heat. This structure functionalized with organic and inorganic groups Thanks to this, many nanometer materials are made. The properties of these materials are typical Much better than polymer and ceramic. Besides all of this, silseskioxanes have various Antimicrobial derivatives are also synthesized by functionalization reactions.

Modern nanoteknolojide farkli bir alan açan Polihedral Oligomerik Silseskioksan molekülleri hem monomerik hem de polimerik yapilarin güçlendirilmesi için yeni bir kimyasal malzeme olarak ortaya çikmaktadir. POSS monomerleri içeren polimerler, termal ve mekanik özelliklerinin iyilestirilmesinden dolayi birçok çalismaya konu olmaktadir. Polihedral Oligomerik Silseskioksan molekülleri, üç boyutuda nanometre seviyesinde olan kübik sekilli dolgu malzemesidir. Polyhedral Oligomeric Silsesquioxane molecules opening a different field in modern nanotechnology A new chemical material for reinforcing both monomeric and polymeric structures appears as. Polymers containing POSS monomers, thermal and mechanical It has been the subject of many studies due to the improvement of its properties. polyhedral Oligomeric Silsesquioxane molecules are cubic shaped in three dimensions at the nanometer level. is the filling material.

Mevcut teknikte POSS nano fazlar, hafif ve yüksek basarimli hibrit nano kompozitlerin hazirlanmasi için tasarlanmaktadir. POSS-güçlendirilmis nanokompozitlerde basarim bölgesi, polimer ve seramik bölgenin arasindadir. POSS yapilarin en önemli iki özelliginden ilki, (POSS) silika (Si02) ve silikon (R2SIO) arasinda, moleküler boyutlari yaklasik olarak 1-3 nm olan küresel sekilli hibrit yapilardir. Bu büyüklükteki POSS molekülü, moleküler boyutta tüm polimerik yapilarin zincirlerinin arasina çok rahat girebilmekte ve polimer matrisi buna bagli olarak güçlendirmektedir (4). In the current art, POSS nanophases are used to make light and high performance hybrid nanocomposites. It is designed to be prepared. Success in POSS-reinforced nanocomposites region is between the polymer and ceramic region. POSS is one of the two most important features of structures. first, (POSS) is between silica (SiO2) and silicon (R2SIO), with molecular sizes of approximately 1-3 nm are spherical shaped hybrid structures. POSS molecule of this size It can easily enter between the chains of all polymeric structures and the polymer matrix accordingly strengthens (4).

Bununla birlikte silika, silikon ve diger dolgularin tersine, herhangi bir POSS molekülü kendisini polimer, biyolojik sistemler veya yüzeyler ile uyumlu hale getiren organik gruplar içermektedir. Siradan organik bilesimlerin tersine, uçucu organik bilesikler salmadiklari için kokusuz ve çevre dostu olarak bilinmektedirler (5). However, unlike silica, silicone and other fillers, any POSS molecule organic groups that make them compatible with polymers, biological systems or surfaces contains. Because they do not release volatile organic compounds, unlike ordinary organic compounds they are known to be odorless and environmentally friendly (5).

Teknigin bilinen durumunda farkli POSS kimyasallari hazirlanmaktadir. POSS molekülü bir veya birkaç tepkin organik grup islevselligi içerebilmektedir. Bu nedenle POSS molekülleri bilinen polimerlere kopolimerizasyon, asilama veya karistirma ile ilave edilebilmektedir. In the state of the art, different POSS chemicals are prepared. POSS molecule is a or it may contain several reactive organic groups functionality. Therefore, POSS molecules It can be added to known polymers by copolymerization, grafting or mixing.

POSS güçlendirilmis nanokompozitler isil dayanimlari nedeniyle yüksek sicakliklarda kullanilabilmektedir. Ayrica, oksidasyon kararli, mekanik özellikleri yüksekt, alev alma özelligi ve açiga çikan isi miktari az, islem viskoziteleri düsüktür. Metakrilat, stiren, norbornen, etilen, epoksit ve siloksanlarin termoplastik ve termoset özellikleri POSS molekülleri kullanilarak iyilestirilebilmektedir (6). POSS reinforced nanocomposites are resistant to high temperatures due to their thermal resistance. can be used. Also, oxidation stable, high mechanical properties, flammability and the amount of heat released is low, and the process viscosities are low. methacrylate, styrene, norbornene, ethylene, Thermoplastic and thermosetting properties of epoxides and siloxanes were evaluated using POSS molecules. can be improved (6).

Konvensiyonel olarak, metal nanoparçaciklari, soy metallerin çesitli tuzlarinin çesitli yöntemlerle indirgenmesi sayesinde sentezlenmektedir. Küresel formlu nanoparçaciklarin geleneksel olarak sentezlenmesi için, sodyum sitrat ya da sodyum borohidrür ile indirgenme islemi kullanilmaktadir. Bunun yaninda metal tuzlarinin UV isik ile fotoindirgenmesi bir diger nanoparçacik elde etme yöntemidir. Conventionally, metal nanoparticles are composed of various salts of noble metals. synthesized by reduction methods. Spherical nanoparticles conventionally reduced by sodium citrate or sodium borohydride to synthesize name is used. In addition, photoreduction of metal salts with UV light is another It is a method of obtaining nanoparticles.

Yüksek serbest yüzey enerjisinden ötürü, metal nanoparçaciklarin kolaylikla kümeleniyor olmasi ve termodinamik açidan kararsiz parçaciklarin formülasyonda dagilmasi büyük bir problem olmakla birlikte, bu problemi asmak ve kararli parçaciklar elde etmek için çesitli yöntemler kullanilmaktadir. Bunlara örnek olarak; sitrat indirgenmesi, tiyol stabilizasyon ve tiyoller, aminler, miseller, dendrimer ve polimerlerin kullanildigi çesitli termal ve fotokimyasal teknikler gösterilebilmektedir. Due to the high free surface energy, metal nanoparticles agglomerate easily. and the dispersion of thermodynamically unstable particles in the formulation is of great importance. However, there are various methods to overcome this problem and obtain stable particles. methods are used. As an example of these; citrate reduction, thiol stabilization and Various thermal and photochemical processes using thiols, amines, micelles, dendrimers and polymers techniques are shown.

Gümüs nanoparçaciklarinin büyüklügü ve seklinin kontrolü büyük bir öneme sahiptir. Çünkü belirli sekil ve büyüklük, optik, elektronik ve katalitik islemlerde önemlidir. Ozellikle optik özellikleri parçacik sekline bagli oldugundan, gümüs nanoparçaciklarinin kompozitlerde bulunmasi, biyo/nanotip, sensör, katalizör ve nanoteknoloji açisindan önemli olmaktadir. Controlling the size and shape of silver nanoparticles is of great importance. because Certain shape and size are important in optical, electronic and catalytic processes. especially optics Since the properties of silver nanoparticles depend on the particle shape, it is possible to use silver nanoparticles in composites. It is important in terms of bio/nanotype, sensor, catalyst and nanotechnology.

Altin nanoparçaciklarin parçacik sekil ve boyutlari ise, UV-VIS spektrumlari incelenerek tayin edilebilmektedir ve yüzey plazmon bant etkisiyle 420-450 nm dalgaboyunda veya parçacik boyutuna göre, daha az ya da daha fazla dalgaboyunda bir absorpsiyon gözlenmektedir. The particle shape and size of gold nanoparticles can be determined by examining their UV-VIS spectra. and the surface plasmon band effect at a wavelength of 420-450 nm or particle Depending on the size, an absorption is observed at less or more wavelengths.

Literatürdeki çalismalar incelendiginde, POSS-TX yapisinda bir fotobaslaticinin sentezlenmedigi ve benzeri tiyokzanton-POSS yapisina sahip bir fotobaslatici kullanilarak fotokimyasal olarak gümüs nanoparçaçiklarin olusturulmadigi gözlemlenmektedir. POSS ve fotobaslatici karisimlarina yönelik çalismalar elektronik endüstrisi, biyomühendislik ve polimer endüstirisi gibi çesitli alanlarda yeni malzemelerin tasarlanmasina yönelik yürütülmektedir. When the studies in the literature are examined, it is seen that a photoinitiator in POSS-TX structure not synthesized and using a photoinitiator with a similar thioxantone-POSS structure. It is observed that silver nanoparticles are not formed photochemically. POSS and Studies on photoinitiator mixtures are in the electronics industry, bioengineering and for the design of new materials in various fields such as the polymer industry is being carried out.

Sonuç olarak yukarida bahsedilen olumsuzluklardan ve eksikliklerden dolayi, ilgili teknik alanda bir yenilik yapma ihtiyaci ortaya çikmistir. As a result, due to the above-mentioned disadvantages and shortcomings, the relevant technical There is a need for innovation in the field.

Bulusun Amaci Mevcut bulus, yukarida bahsedilen gereksinimleri karsilayan, tüm dezavantajlari ortadan kaldiran ve ilave bazi avantajlar getiren, POSS-TX nanofotobaslaticinin sentezi ve POSS-TX yardimi ile yerinde fotokimyasal olarak Ag nanoparçacik sentezi ve kirisik yüzey olusumu ile Bulusun amaci, Polioligosilseskioksan grubu tasiyan tiyokzanton türevi fotobaslatici sentezlemektir. Purpose of the Invention The present invention satisfies the above-mentioned requirements, eliminates all disadvantages. Synthesis of POSS-TX nanophotoinitiator and POSS-TX With the help of in situ photochemical Ag nanoparticle synthesis and wrinkled surface formation. The aim of the invention is to introduce a thioxantone derivative photoinitiator carrying the polyoligosylsesquioxane group. is to synthesize.

Bulusun bir diger amaci, sentezlenen fotobaslaticiyi kullanarak gümüs nanoparçaciklar elde etmektir. Another object of the invention is to obtain silver nanoparticles using the synthesized photoinitiator. is to do.

Bulusun amaci, in-situ olarak kendiliginden düzenleme gerçeklesmis ve nanoboyutlu gümüs nanoparçaciklari içeren bir kirisik yüzey çok kisa sürede ve yüksek verimle elde etmektir. The aim of the invention is to achieve in-situ self-regulation and nanosized silver It is to obtain a wrinkled surface containing nanoparticles in a very short time and with high efficiency.

Bulusun bir amaci, yerinde tek kap yöntemiyle hizli bir sekilde kirisik ve antibakteriyel bir yüzey elde etmektir. It is an object of the invention to rapidly produce an anti-wrinkle and antibacterial treatment by the in-situ one-pot method. to obtain a surface.

Bulusun yapisal ve karakteristik özellikleri ve tüm avantajlari asagida verilen detayli açiklama sayesinde daha net olarak anlasilacaktir ve bu nedenle degerlendirmenin de bu detayli açiklama göz önüne alinarak yapilmasi gerekmektedir. The structural and characteristic features of the invention and all its advantages are described in detail below. will be more clearly understood by means of must be made taking into account the description.

Bulusun Detayli Açiklamasi Bu detayli açiklamada, in-situ olarak kendiliginden düzenleme gerçeklesmis ve nanoboyutlu gümüs nanoparçaciklari içeren kirisik bir yüzey elde edilmesi, sadece konunun daha iyi anlasilmasina yönelik olarak ve hiçbir sinirlayici etki olusturmayacak sekilde açiklanmaktadir. Detailed Description of the Invention In this detailed explanation, in-situ self-regulation has taken place and nanoscale obtaining a wrinkled surface containing silver nanoparticles will only make the subject matter better. for understanding and without any limiting effect is explained.

Bulus, Polioligosilseskioksan (POSS) yapisina sahip fotobaslaticilarin sentezlenmesi ve bu fotobaslaticilar kullanilarak fotopolimerizasyonlarin gerçeklestirilmesi ve POSS yapisini içeren polimer matriksinde Ag nanoparçaciklarin es zamanli ve in-situ sentezi sonucunda kirisik yüzeylerin elde edilme y'ontemi ilgilidir. Söz konusu bulusta, baslatici olarak bulus kapsaminda sentezlenen POSS, monomer olarak da PEGMA-PEGDA kullanilmaktadir. The invention is to synthesize photoinitiators with polyoligosylsesquioxane (POSS) structure and realization of photopolymerizations and POSS structure using photoinitiators As a result of the simultaneous and in-situ synthesis of Ag nanoparticles in the polymer matrix containing The method of obtaining the creased surfaces is relevant. In the invention in question, the invention as the initiator POSS synthesized within the scope of the study is used as a monomer as well as PEGMA-PEGDA.

Gümüs iyonlarinin in-situ olarak gümüs nanoparçaciklara indirgenmesi fotopolimerisazyon yöntemi ile gerçeklestirilmektedir. In-situ reduction of silver ions to silver nanoparticles photopolymerization carried out by the method.

POSS-TX fotobaslatici sentezi o 2-(karboksimetoksi)tiyoksanton (TX-OCHZCOOH) bilesigi tiyosalisik asit kullanilarak o Saflastirilan bilesik ile 2-[(9-Okso-9H-tiyoksanton-2-il)oksi]asetil klorür (TX- OCH2COCI) bilesigi Tiyonil klorür reaktifinden yararlanilarak sentezlenir ve elde edilen bilesigin yapisi FTIR, 1H-NMR, APT spektrumlarindan yararlanilarak aydinlatilir, o TX-OCHZCOCl bilesigi ile amino-izopropil POSS bilesiginin reaksiyonu sonucunda POSS-TX fotobaslatici sentezlenir ve bilesigin yapisi FTIR, 1H-NMR, APT spektrumlarindan yararlanilarak aydinlatilir. POSS-TX photoinitiator synthesis o 2-(carboxymethoxy)thioxantone (TX-OCHZCOOH) compound using thiosalisic acid o 2-[(9-Oxo-9H-thioxanton-2-yl)oxy]acetyl chloride (TX- OCH2COCI) is synthesized using the thionyl chloride reagent and obtained. The structure of the obtained compound was determined by using the FTIR, 1H-NMR, APT spectra. is illuminated, o As a result of the reaction of the TX-OCHZCOCl compound and the amino-isopropyl POSS compound The POSS-TX photoinitiator is synthesized and the structure of the compound is FTIR, 1H-NMR, APT illuminated using spectra.

Gümüs nanoparçacik ve kirisik yüzey elde etme yöntemi, formülasyon kullanilarak solüsyon hazirlanmasi ve hazirlanan solüsyon vasitasiyla nanokompozit film elde edilmesi islem basamaklarini içermektedir. The method of obtaining silver nanoparticles and wrinkled surface, solution using formulation preparation and obtaining nanocomposite film by means of the prepared solution. includes steps.

Bahsedilen formülasyonda çapraz bagli polimeri hazirlamak için, akrilik bazli oligomer ve akrilik bazli monomer olarak, poli(etilen glikol) diakrilat, poli(etilen glikol) monoakrilat, poli(etilen glikol) metil eter akrilat, kullanilmaktadir. To prepare the cross-linked polymer in the mentioned formulation, acrylic-based oligomer and as acrylic-based monomer, poly(ethylene glycol) diacrylate, poly(ethylene glycol) monoacrylate, poly(ethylene glycol) methyl ether acrylate is used.

Formülasvon kullanilarak solüsyon hazirlanmasi: POSS-TX ve AGN03 oda sicakliginda bir beher içerisine koyulur, Akrilik bazli oligomer ve monomer behere ilave edilir, Elde edilen akrilik bazli karisim yaklasik 15 dakika süresince oda sicakliginda ultrasonik banyoya birakilir, Akrilik bazli karisimi homojen hale getirmek üzere, prob tipli ultrasonik karistiricida yaklasik 2 saniye karistirilir, Son asamada ultrasonik banyo ile degas elde edilir. Preparation of solution using formulation: POSS-TX and AGN03 are placed in a beaker at room temperature, Acrylic-based oligomer and monomer are added to the beaker, The resulting acrylic-based mixture is kept at room temperature for about 15 minutes. left in an ultrasonic bath, In the probe type ultrasonic mixer to homogenize the acrylic-based mixture. mixed for about 2 seconds, In the last stage, degas is obtained by ultrasonic bath.

Hazirlanan solüsyon vasitasiyla nanokompozit film elde edilmesi: Elde edilen solüsyon, 40 mikrometre kalinlikta olacak sekilde cam plaka üzerine kaplanir, Cam plaka üzerine kaplanan solüsyon UV-kürlestirme cihazi vasitasiyla, UV isigina maruz birakilir. kapsaminda sentezlenen POSS kafesine sahip fotobaslatici, polimerizasyonun gerçeklesmesinde ve kirisik yüzey olusumunda önemli bir role sahiptir. Ag nanoparçacik sentezi ile, Ag tuzundan fotobaslatici beraberinde Ag nanoparçaciklarin POSS kafesinde kendiginden düzenlenmesi ve antibakteriyel yüzey özelligi saglanmaktadir. Obtaining nanocomposite film with the prepared solution: The resulting solution is poured onto a glass plate with a thickness of 40 micrometers. is covered, The solution coated on the glass plate is exposed to UV light by means of the UV-curing device. be exposed. The photoinitiator with the POSS cage synthesized within the scope of It has an important role in the realization of the formation and the formation of the wrinkled surface. Ag nanoparticle With the synthesis of Ag salt in the POSS lattice of Ag nanoparticles along with the photoinitiator It provides self-regulation and antibacterial surface properties.

Bulus konusu yöntemin islem adimlarindan bir olan fotokimyasal aydinlatma yöntemini olusturan aydinlatma zamani ve isik yogunlugunun, yüzey özelliklerine ve nanoparçacik olusumuna katkisi bulunmaktadir. Photochemical lighting method, which is one of the processing steps of the method of the invention. illumination time and light intensity, surface properties and nanoparticle contributes to its formation.

Nanokompozit malzeme içerisindeki gümüs nanoparçaciklarin karakterizasyonu UV-VIS spektrumlari ile belirlenmektedir. Spektrum incelendiginde; gümüs nanoparçaciklari 420-450 nm arasinda absorpsiyon yapmaktadir. Gümüs nanoparçaciklarin elde edilen absorpsiyon degerleri, literatürde var olan degerlere benzer olarak elde edilmektedir. Characterization of silver nanoparticles in nanocomposite material UV-VIS determined by the spectra. When the spectrum is examined; silver nanoparticles 420-450 It absorbs between nm. The resulting absorption of silver nanoparticles values are obtained similar to the values available in the literature.

SEM diyagrami incelendiginde ise; kirisik yüzey olusumu ve Ag nanoparçaciklarin POSS kafesini içeren polimer matriksinde düzgün sekilli olarak dagildigi görülmektedir. When the SEM diagram is examined; Wrinkled surface formation and POSS of Ag nanoparticles It is seen that it is distributed uniformly in the polymer matrix containing the lattice.

Söz konusu bulus ile POSS yapisini içeren polimer matriksinde Ag nanoparçaciklarin es zamanli ve in-situ sentezi sonucunda kirisik yüzeylerin elde edilmis ve SEM grafikleri ve UV- Vis sonuçlari ile kirisik yüzeylerin elde edilmesi dogrulanmistir. With the invention in question, Ag nanoparticles are identical in the polymer matrix containing the POSS structure. As a result of time and in-situ synthesis, the wrinkled surfaces were obtained and SEM graphics and UV- Obtaining the wrinkled surfaces was confirmed by the Vis results.

KAYNAKLAR 1) Guizhi Li, Lichang Wang; Pittman, Jr., Charles U. (2001). "Polyhedral Oligomeric Silsesquioxane (POSS): a Review". Journal of lnorganic and Organometallic Polymers 11 (3): 2) Layer-by-layer assembly of Ru3+ and Si80208- into electrochemically active silicate films, Rassaei, L; Sillanpaa, M; Milsom, EV, et al., Journal of solid state electrochemistry 12 (2008) 747-755. 3) Wang, X.; Ervithayasupom, V.; Zhang Y.; Kawakami, Y. (201 l). "Reversible self- assembly of dendrimer based on polyhedral Oligomeric silsesquioxanes (POSS)". Chemical Communications 47: 1282. RESOURCES 1) Guizhi Li, Lichang Wang; Pittman, Jr., Charles U. (2001). "Polyhedral Oligomeric Silsesquioxane (POSS): a Review". Journal of Inorganic and Organometallic Polymers 11 (3): 2) Layer-by-layer assembly of Ru3+ and Si80208- into electrochemically active silicate films, Rassai, L; Sillanpaa, M; Milsom, EV, et al., Journal of solid state electrochemistry 12 (2008) 747-755. 3) Wang, X.; Ervithayasupom, V.; Zhang Y.; Kawakami, Y. (201 l). "Reversible self- assembly of dendrimer based on polyhedral Oligomeric silsesquioxanes (POSS)". Chemical Communications 47:1282.

) Li, G., Wang, L., Hanli, Ni, Pittman, C.U., (2001). “Polyhedral Oligomeric Silsesquioxane (POSS) Polymers and Copolymers” 6) Kuo, S.W., Chang, PC., (2011). “POSS Related Polymer Nanocomposites” ) Li, G., Wang, L., Hanli, Ni, Pittman, C.U., (2001). “Polyhedral Oligomeric Silsesquioxane (POSS) Polymers and Copolymers” 6) Kuo, S.W., Chang, PC., (2011). “POSS Related Polymer Nanocomposites”

Claims (4)

ISTEMLERREQUESTS 1. Esnek elektronik malzeme ve optik cihazlarda kullanilmak üzere, yerinde tek kap yöntemiyle hizli bir sekilde antibakteriyel ve kirisik bir yüzey elde etme yöntemi olup, özelligi; 2-(karb0ksimetoksi)tiy0kzant0n bilesiginin tiyosalisik asit kullanilarak sentezlenmesi ve saflastirilmasi, saflastirilan bilesik ile Tiyonil klorür reaktifinden yararlanilarak 2-[(9-Okso-9H- tiyoksanton-2-il)oksi]asetil klorür bilesiginin sentezlenmesi, 2-[(9-Okso-9H-tiyoksanton-2-il)0ksi]asetiI klorür bilesigi ile amino-izopropil POSS bilesiginin reaksiyonu sonucunda POSS-TX fotobaslatici sentezlenmesi, POSS-TX ve gümüs nitratin oda sicakliginda bir beher içerisine koyulmasi, akrilik bazli oligomer ve monomerin behere ilave edilmesi, elde edilen akrilik bazli karisimin ultrasonik banyoya birakilmasi, akrilik bazli karisimi homojen hale getirmek üzere, prob tipli ultrasonik karistiricida karistirilmasi, ultrasonik banyo ile degas elde edilmesi, elde edilen solüsyonun, 40 mikrometre kalinlikta olacak sekilde cam plaka üzerine kaplanmasi, cam plaka üzerine kaplanan solüsyonun UV-kürlestirme cihazi vasitasiyla, UV isigina maruz birakilmasi, islem adimlarini içermesidir.1. It is a method of obtaining an antibacterial and wrinkled surface quickly with the single cup method in place, to be used in flexible electronic materials and optical devices, and its feature is; Synthesis and purification of 2-(carboxymethoxy)thioxanthone compound using thiosalisic acid, synthesis of 2-[(9-Oxo-9H-thioxanton-2-yl)oxy]acetyl chloride compound using the purified compound and Thionyl chloride reagent, 2-[(9- Synthesis of POSS-TX photoinitiator as a result of the reaction of oxo-9H-thioxanton-2-yl)Oxy]acetyl chloride compound and amino-isopropyl POSS compound, placing POSS-TX and silver nitrate in a beaker at room temperature, adding acrylic-based oligomer and monomer to the beaker , pouring the obtained acrylic-based mixture into an ultrasonic bath, mixing it in a probe-type ultrasonic mixer to make the acrylic-based mixture homogeneous, obtaining degas with an ultrasonic bath, coating the obtained solution on a glass plate with a thickness of 40 micrometers, the solution coated on the glass plate Exposure to UV light, via the UV-curing device, includes the processing steps. 2. Istem 1ie uygun antibakteriyel ve kirisik bir yüzey elde etme yöntem olup, özelligi; e islem adiminda bahsedilen akrilik bazli oligomer ve monomer, poli(etilen glikol) diakrilat, poli(etilen glikol) monoakrilat ve poli(etilen glikol) metil eter akrilattir.2. It is a method of obtaining an antibacterial and wrinkled surface in accordance with claim 1, and its feature is; The acrylic-based oligomer and monomer mentioned in the e process step are poly(ethylene glycol) diacrylate, poly(ethylene glycol) monoacrylate and poly(ethylene glycol) methyl ether acrylate. 3. Istem 1' e uygun antibakteriyel ve kirisik bir yüzey elde etme yöntem olup özelligi; f islem adiminda bahsedilen ultrasonik banyoya birakma isleminin oda sicakliginda yaklasik 153. It is the method of obtaining an antibacterial and wrinkled surface in accordance with claim 1, and its feature is; The process of leaving the ultrasonic bath mentioned in the f process step is about 15 minutes at room temperature. 4. Istem 1' e uygun antibakteriyel ve kirisik bir yüzey elde etme yöntem olup özelligi; g islem adiminda bahsedilen karistirma isleminin yaklasik 2 saniye yapilmasidir.4. It is the method of obtaining an antibacterial and wrinkled surface in accordance with claim 1, and its feature is; The mixing process mentioned in the g process step is to be done for about 2 seconds.
TR2017/22696A 2017-12-28 2017-12-28 Synthesis of POSS-TX Nanophoto Initiator TR201722696A2 (en)

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Application Number Priority Date Filing Date Title
TR2017/22696A TR201722696A2 (en) 2017-12-28 2017-12-28 Synthesis of POSS-TX Nanophoto Initiator
US16/957,622 US11591418B2 (en) 2017-12-28 2018-12-28 POSS-TX nano-photo-initiator synthesis and in situ photochemical Ag nano-particle synthesis with the help of POSS-TX and wrinkled surface formation
PCT/TR2018/050924 WO2019132848A1 (en) 2017-12-28 2018-12-28 Poss-tx nano-photo-initiator synthesis and in situ photochemical ag nano-particle synthesis with the help of poss-tx and wrinkled surface formation
DE112018006657.6T DE112018006657B4 (en) 2017-12-28 2018-12-28 Method for producing an antibacterial and anti-wrinkle surface, nanocomposite surfaces produced with the method and the use of the nanocomposite surfaces

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