TW201516195A - Aluminum nitride fiber and preparation method thereof and highly thermal conductive composite material - Google Patents
Aluminum nitride fiber and preparation method thereof and highly thermal conductive composite material Download PDFInfo
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本發明是有關於一種高散熱纖維及其製備方法,及含有該高散熱纖維的高分子複合材料,特別是指一種氮化鋁纖維及其製備方法,以及含有該氮化鋁纖維的高導熱複合材料。 The invention relates to a high heat dissipating fiber and a preparation method thereof, and a polymer composite material containing the high heat dissipating fiber, in particular to an aluminum nitride fiber and a preparation method thereof, and a high thermal conductive composite containing the aluminum nitride fiber material.
高導熱性高分子複合材料是目前被廣泛使用於電子元件導熱的高性能材料之一,而絕緣高導熱高分子複合材料,則通常是在高分子材料中添加具有高熱傳導性質的無機填充劑,例如陶瓷粉體,而達成絕緣、散熱的目的。其中,氮化鋁因具有高熱傳導係數(理論值:320W/mK)、良好的電絕緣性、低介電常數與介電損失率,因此成為高散熱性陶瓷粉體的主要代表之一。 The high thermal conductivity polymer composite material is one of the high performance materials widely used in the thermal conduction of electronic components, and the insulating high thermal conductivity polymer composite material is usually added with an inorganic filler having high thermal conductivity in the polymer material. For example, ceramic powder, to achieve the purpose of insulation and heat dissipation. Among them, aluminum nitride is one of the main representatives of high heat dissipation ceramic powder because of its high thermal conductivity (theoretical value: 320 W/mK), good electrical insulation, low dielectric constant and dielectric loss.
熱傳導是透過物質間的直接接觸,將「熱」由高溫區域傳向低溫區域的一種熱傳遞的方式。而高分子的結構一般是屬於飽和體系,無自由電子存在,分子運動困難,所以高分子材料本身的熱傳導主要是晶格振動的結果,因此熱傳導效果不佳。故,為了得到絕緣且具有高導熱性的高分子材料,目前大都是藉由添加具有高熱傳導性質 的無機粉體於高分子材料中,如前述的氮化鋁粉體,以達到絕緣及散熱的目的。 Heat conduction is a way of transferring heat from a high temperature zone to a low temperature zone through direct contact between materials. The structure of the polymer generally belongs to a saturated system. There is no free electron and the molecular motion is difficult. Therefore, the heat conduction of the polymer material itself is mainly the result of lattice vibration, so the heat conduction effect is not good. Therefore, in order to obtain a polymer material having high thermal conductivity and insulation, most of them are currently highly thermally conductive. The inorganic powder is used in a polymer material, such as the aforementioned aluminum nitride powder, for the purpose of insulation and heat dissipation.
然而,於高分子材料中添加氮化鋁粉體雖然可以增加導熱性,但是氮化鋁粉體的添加量與熱傳導能力及加工性有高度的關聯性;添加量太少,無法形成熱傳遞的通路,導致熱傳導能力不佳;添加太多,不但成本提高外,還會造成加工塑形的困難度。例如,一般為了得到具有高散熱性的絕緣複合材料,氮化鋁粉體的添加量都不小於50%,甚至為了得到散熱性大於70W/mK的絕緣散熱材料,氮化鋁粉體的添加量還會高於75%,不僅成本提高,也造成加工塑形的難度。 However, the addition of the aluminum nitride powder to the polymer material can increase the thermal conductivity, but the addition amount of the aluminum nitride powder is highly correlated with the heat transfer ability and the processability; the amount of addition is too small to form heat transfer. The passage leads to poor heat transfer capacity; too much addition, not only increases the cost, but also causes difficulty in processing and shaping. For example, in general, in order to obtain an insulating composite material having high heat dissipation properties, the amount of aluminum nitride powder added is not less than 50%, and even in order to obtain an insulating heat dissipating material having heat dissipation of more than 70 W/mK, the amount of aluminum nitride powder is added. It will be higher than 75%, which not only increases the cost, but also makes it difficult to process and shape.
因此,如何讓氮化鋁粉體可以在高分子基材中形成良好的熱傳導通路,使其可以降低添加量,讓高分子複合材料可以具有良好的導熱性但不影響原高分子材料的特性,則為發明人努力研究開發的重要方向。 Therefore, how to make the aluminum nitride powder form a good heat conduction path in the polymer substrate, so that the addition amount can be reduced, and the polymer composite material can have good thermal conductivity without affecting the characteristics of the original polymer material. It is an important direction for the inventors to study and develop.
因此,本發明之目的,即在提供一種具有高導熱性的氮化鋁纖維的製備方法。 Accordingly, it is an object of the present invention to provide a method of preparing an aluminum nitride fiber having high thermal conductivity.
此外,本發明的另一目的,即在提供一種具有高導熱性的氮化鋁纖維。 Further, another object of the present invention is to provide an aluminum nitride fiber having high thermal conductivity.
又,本發明的又一目的,即在提供一種具有氮化鋁纖維的高導熱複合材料。 Still another object of the present invention is to provide a highly thermally conductive composite material having aluminum nitride fibers.
於是,本發明一種具有高導熱性的氮化鋁纖維的製備方法包含以下3個步驟。 Thus, the method for preparing an aluminum nitride fiber having high thermal conductivity of the present invention comprises the following three steps.
(a)準備一紡絲液,該紡絲液的組成分包括一氮化鋁粉末、一含鋁的前驅物、一溶劑,及一高分子增稠劑,其中,以該紡絲液的重量百分比為100wt%計,該氮化鋁粉末的重量百分比介於2~20wt%,且該含鋁的前驅物與氮化鋁粉末的重量比值介於25~55。 (a) preparing a spinning solution, the spinning composition comprising an aluminum nitride powder, an aluminum-containing precursor, a solvent, and a polymeric thickener, wherein the weight of the spinning solution The percentage by weight is 100% by weight, the weight percentage of the aluminum nitride powder is between 2 and 20% by weight, and the weight ratio of the aluminum-containing precursor to the aluminum nitride powder is between 25 and 55.
(b)將該紡絲液利用紡絲方法製成含有氮化鋁的高分子複合纖維。 (b) The spinning solution is formed into a polymer composite fiber containing aluminum nitride by a spinning method.
(c)將該高分子複合纖維於400~550℃、惰性氣氛下進行煅燒,令該高分子複合纖維的有機物成分於煅燒過程被移除,即可得到氮化鋁纖維。 (c) The polymer composite fiber is calcined at 400 to 550 ° C in an inert atmosphere, and the organic component of the polymer composite fiber is removed in the calcination process to obtain an aluminum nitride fiber.
此外,本發明一種具有高導熱性的氮化鋁纖維,該氮化鋁纖維是由如前所述的該氮化鋁纖維的製備方法所製得,且該氮化鋁纖維的長/徑比大於50。 In addition, the present invention provides an aluminum nitride fiber having high thermal conductivity, which is obtained by the method for preparing the aluminum nitride fiber as described above, and the length/diameter ratio of the aluminum nitride fiber. More than 50.
又,本發明一種具有氮化鋁纖維的高導熱複合材料,包含一基材及多條分散於該基材的氮化鋁纖維,該基材選自高分子材料,該些氮化鋁纖維是由如前所述的該氮化鋁纖維的製備方法所製得。 Moreover, the present invention provides a highly thermally conductive composite material having aluminum nitride fibers, comprising a substrate and a plurality of aluminum nitride fibers dispersed on the substrate, the substrate being selected from the group consisting of polymer materials, and the aluminum nitride fibers are It is produced by the method for producing the aluminum nitride fiber as described above.
21‧‧‧步驟 21‧‧‧Steps
22‧‧‧步驟 22‧‧‧Steps
23‧‧‧步驟 23‧‧‧Steps
本發明之其他的特徵及功效,將於參照圖式的實施方式中清楚地呈現,其中:圖1是一流程圖,說明本發明氮化鋁纖維的製備方法的該較佳實施例;圖2是一SEM照片,說明本發明該較佳實施例製得之氮化鋁纖維;及 圖3是一XRD光譜,說明由本發明該較佳實施例製得之氮化鋁纖維的XRD量測結果。 Other features and effects of the present invention will be apparent from the following description of the drawings. FIG. 1 is a flow chart illustrating the preferred embodiment of the method for preparing aluminum nitride fibers of the present invention; Is an SEM photograph illustrating the aluminum nitride fiber produced by the preferred embodiment of the present invention; and Figure 3 is an XRD spectrum illustrating the XRD measurement results of the aluminum nitride fibers produced by the preferred embodiment of the present invention.
有關本發明之前述及其他技術內容、特點與功效,在以下配合參考圖式之一個較佳實施例的詳細說明中,將可清楚的呈現。 The above and other technical contents, features and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments.
本發明一種氮化鋁纖維的製備方法的該較佳實施例是用以製作一種具有高散熱性的氮化鋁纖維,且較佳地,該氮化鋁纖維的長/徑比大於50。 The preferred embodiment of the method for producing an aluminum nitride fiber of the present invention is for producing an aluminum nitride fiber having high heat dissipation properties, and preferably, the aluminum nitride fiber has a length/diameter ratio of more than 50.
參閱圖1,本發明該氮化鋁纖維的製備方法的該較佳實施例,是包含以下3個步驟。 Referring to Figure 1, the preferred embodiment of the method for preparing the aluminum nitride fiber of the present invention comprises the following three steps.
步驟21,準備一紡絲液。 In step 21, a spinning solution is prepared.
該紡絲液的組成分包括一氮化鋁粉末、一含鋁的前驅物、一溶劑,及一高分子增稠劑。 The composition of the spinning solution includes an aluminum nitride powder, an aluminum-containing precursor, a solvent, and a polymeric thickener.
該含鋁的前驅物選自氯化鋁、氫氧化鋁、氧化鋁,及前述其中一組合,該溶劑則選自對該紡絲液中其它成分有較佳分散性及溶解性的溶劑,例如:乙醇、異丙醇、丙酮等;該高分子增稠劑選自聚乙烯醇、海藻酸鈉、聚烷氧乙烯、聚乙烯醇縮丁醛、乙基纖維素、聚乙烯基吡咯烷酮,及前述其中一組合。 The aluminum-containing precursor is selected from the group consisting of aluminum chloride, aluminum hydroxide, aluminum oxide, and a combination of the foregoing, the solvent being selected from solvents having better dispersibility and solubility for other components in the spinning solution, such as : ethanol, isopropanol, acetone, etc.; the polymeric thickener is selected from the group consisting of polyvinyl alcohol, sodium alginate, polyalkoxyethylene, polyvinyl butyral, ethyl cellulose, polyvinyl pyrrolidone, and the foregoing One of the combinations.
要說明的是,該紡絲液中各成分的比例控制是決定後續形成之氮化鋁纖維品質的重要關鍵因素,當紡絲液中氮化鋁含量不足,則形成之氮化鋁纖維的品質不佳而會影響導熱性,而當紡絲液中的氮化鋁粉末過多、高分子 增稠劑不足或是黏度過高時,則在紡絲階段會有不易成型或形成團聚物,反而會有散熱性降低的缺點產生;較佳地,為了讓該紡絲液於後續紡絲過程中可順利形成高分子複合纖維及品質良好的氮化鋁纖維,該紡絲液的黏度是控制在70~140cps,且以該紡絲液的重量百分比為100wt%計,該氮化鋁粉末的重量百分比介於2~20wt%,該高分子增稠劑的的重量百分比介於5~15wt%,且該含鋁的前驅物與氮化鋁粉末的重量比值介於25~55;較佳地,該氮化鋁粉末的重量百分比介於3~10%,該高分子增稠劑的的重量百分比介於10~15wt%,且該含鋁的前驅物與氮化鋁粉末的重量比值介於25~40。 It should be noted that the proportional control of the components in the spinning solution is an important key factor determining the quality of the subsequently formed aluminum nitride fiber. When the content of aluminum nitride in the spinning solution is insufficient, the quality of the formed aluminum nitride fiber is Poor, it will affect the thermal conductivity, and when the aluminum nitride powder in the spinning solution is too much, the polymer When the thickener is insufficient or the viscosity is too high, there is a disadvantage that it is difficult to form or form agglomerates during the spinning stage, and there is a disadvantage that the heat dissipation is lowered; preferably, in order to allow the spinning solution to be in the subsequent spinning process The polymer composite fiber and the aluminum nitride fiber of good quality can be smoothly formed, and the viscosity of the spinning solution is controlled at 70 to 140 cps, and the weight percentage of the spinning solution is 100 wt%, and the aluminum nitride powder is The weight percentage is between 2 and 20% by weight, the weight percentage of the polymeric thickener is between 5 and 15% by weight, and the weight ratio of the aluminum-containing precursor to the aluminum nitride powder is between 25 and 55; preferably The weight percentage of the aluminum nitride powder is between 3 and 10%, the weight percentage of the polymeric thickener is between 10 and 15% by weight, and the weight ratio of the aluminum-containing precursor to the aluminum nitride powder is between 25~40.
接著進行步驟22,製得高分子複合纖維。 Next, in step 22, a polymer composite fiber is obtained.
該步驟22是將該步驟21配置而得的紡絲液利用溶液紡絲方法,例如濕式紡絲方法或是乾式紡絲方法,製成該些含有氮化鋁顆粒的高分子複合纖維。由於該溶液紡絲方法相關參數的調整及控制為本技術領域所知悉,因此不再多加贅述。於本實施例中,該步驟22是以利用電紡絲方法將該紡絲液製成高分子複合纖維為例作說明,茲將該電紡絲製程說明如下。 In the step 22, the spinning solution obtained by disposing the step 21 is formed by a solution spinning method, for example, a wet spinning method or a dry spinning method, to form the polymer composite fibers containing aluminum nitride particles. Since the adjustment and control of the parameters related to the solution spinning method are known in the art, no further description is provided. In the present embodiment, the step 22 is described by taking the spinning solution into a polymer composite fiber by an electrospinning method. The electrospinning process is described below.
首先將該步驟21製得,黏度控制在70~140cps的紡絲液注入一具有不銹鋼針頭的針管中,並設置一遠離該針頭並接地的接收裝置,接著於該針頭施加9~18千伏(kV)的高壓靜電,而於該針頭與接收裝置間產生一個強大的電場,令自該針頭噴向該接收裝置運動的紡絲液加速並 展開成更細小的次微米液柱,並同時令該溶劑揮發,即可在該接收裝置上形成多數非織布狀(non-woven)的高分子複合纖維。 First, the step 21 is prepared, the spinning solution with a viscosity control of 70-140 cps is injected into a needle tube having a stainless steel needle, and a receiving device remote from the needle and grounded is disposed, and then 9 to 18 kV is applied to the needle ( High-voltage static electricity of kV), and a strong electric field is generated between the needle and the receiving device, so that the spinning solution that is sprayed from the needle to the receiving device is accelerated and A plurality of non-woven polymer composite fibers are formed on the receiving device by unfolding into a finer submicron liquid column and simultaneously volatilizing the solvent.
最後進行步驟23,將該些高分子複合纖維進行煅燒,製得氮化鋁纖維。 Finally, in step 23, the polymer composite fibers are calcined to obtain aluminum nitride fibers.
該步驟23是將步驟22製得的該些含有氮化鋁粉末及含鋁的前驅物的高分子複合纖維置於一高溫爐中,於惰性氣氛、及400~500℃的溫度條件下,將該些高分子複合纖維進行煅燒,移除該高分子複合纖維中的有機成分,由於該些高分子複合纖維中的氮化鋁粉末及該含鋁的前驅物於此煅燒過程中會產生氧化物,該氧化物會將氮化鋁粉末包覆起來而形成長鏈狀,因此,於煅燒後即可製得連續的氮化鋁纖維。於本實施例中,是將該些高分子複合纖維在400~500℃、氮氣條件下,煅燒0.5~2小時,而製得該些氮化鋁纖維。 In the step 23, the polymer composite fibers containing the aluminum nitride powder and the aluminum-containing precursor prepared in the step 22 are placed in a high temperature furnace under an inert atmosphere and at a temperature of 400 to 500 ° C. The polymer composite fibers are calcined to remove organic components in the polymer composite fiber, and the aluminum nitride powder and the aluminum-containing precursor in the polymer composite fibers generate oxides during the calcination process. The oxide encapsulates the aluminum nitride powder to form a long chain shape, so that continuous aluminum nitride fiber can be obtained after calcination. In the present embodiment, the high molecular composite fibers are calcined at 400 to 500 ° C under nitrogen for 0.5 to 2 hours to obtain the aluminum nitride fibers.
參閱圖2、圖3,圖2所示為所製得的氮化鋁纖維的掃描式電子顯微鏡(SEM)照片;而圖3則為將該些氮化鋁纖維的XRD檢測結果。該XRD結果經與ICDD資料庫比對後,證實為氮化鋁結構。 Referring to Figures 2 and 3, Figure 2 shows a scanning electron microscope (SEM) photograph of the obtained aluminum nitride fiber; and Figure 3 shows the results of XRD detection of the aluminum nitride fibers. The XRD results were confirmed to be aluminum nitride structures after being compared with the ICDD database.
而將本發明製得之氮化鋁纖維摻雜於一高分子基材中,即可獲得具有高導熱性的高導熱複合材料,之後,將該高導熱複合材料再經由一般高分子加工方式,如壓出或擠壓成型等,即可製成適用於各種用途的散熱元件。 When the aluminum nitride fiber obtained by the invention is doped into a polymer substrate, a highly thermally conductive composite material having high thermal conductivity can be obtained, and then the high thermal conductive composite material is processed through a general polymer processing method. If extruded or extruded, it can be made into a heat dissipating component suitable for various purposes.
前述該高導熱複合材料的該高分子基材可選自 一般熱塑性塑膠或熱固性塑膠,例如:聚乙烯、聚丙烯、聚苯乙烯、聚甲基丙烯酸甲酯、聚碳酸酯、聚對苯二甲酸乙二醇酯,熱固性樹脂:如酚醛樹脂、環氧樹脂、聚醯亞胺、聚酯,或ABS樹脂等,該氮化鋁纖維則可視該高導熱複合材料的導熱要求而加、減其添加量;較佳地,在不影響該高分子基材本身物性並可具有高導熱性的前提下,以該高導熱複合材料的重量為100wt%計,該氮化鋁纖維的添加量為10~50%。 The polymer substrate of the foregoing high thermal conductive composite material may be selected from General thermoplastic or thermosetting plastics, such as: polyethylene, polypropylene, polystyrene, polymethyl methacrylate, polycarbonate, polyethylene terephthalate, thermosetting resin: such as phenolic resin, epoxy resin Polyimide, polyester, or ABS resin, etc., the aluminum nitride fiber may be added or subtracted according to the heat conduction requirement of the high thermal conductive composite material; preferably, the polymer substrate itself is not affected Under the premise of physical properties and high thermal conductivity, the aluminum nitride fiber is added in an amount of 10 to 50% based on 100% by weight of the high thermal conductive composite.
接著以下列1個具體例及1個比較例說明本發明該氮化鋁纖維的製備方法,當可更清楚明白。 Next, the preparation method of the aluminum nitride fiber of the present invention will be described in the following specific examples and one comparative example, which can be more clearly understood.
具體例1 Specific example 1
準備一包括0.15g氮化鋁粉末、5.5g氯化鋁溶液、2g溶劑,及0.6g的聚乙烯醇的紡絲液。 A spinning solution comprising 0.15 g of aluminum nitride powder, 5.5 g of an aluminum chloride solution, 2 g of a solvent, and 0.6 g of polyvinyl alcohol was prepared.
將該紡絲液注入一針頭中,在9千伏(kV)的條件下利用電紡絲方式令該紡絲液形成多數高分子複合纖維。 The spinning solution was poured into a needle, and the spinning solution was formed into a plurality of polymer composite fibers by electrospinning under conditions of 9 kV.
接著將該些高分子複合纖維放入高溫爐中,以450℃的條件煅燒0.5小時,即可得到氮化鋁纖維A-1。 Then, the polymer composite fibers were placed in a high-temperature furnace and calcined at 450 ° C for 0.5 hour to obtain an aluminum nitride fiber A-1.
比較例1 Comparative example 1
該比較例1的製作方式與該具體例1大致相同,不同處在於該比較例1的紡絲液中,氮化鋁粉末為0.7g,氯化鋁溶液為5.5g,可製得氮化鋁纖維B-1。 The production method of Comparative Example 1 was substantially the same as that of the specific example 1, except that in the spinning solution of Comparative Example 1, the aluminum nitride powder was 0.7 g, and the aluminum chloride solution was 5.5 g, and aluminum nitride was obtained. Fiber B-1.
接著分別將前述該具體例1及比較例1製得之氮化鋁纖維和習知常用之氮化鋁粉末摻雜於環氧樹脂高分 子材料中製成不同試片,再利用熱傳導分析儀進行導熱性量測,並將所測得的結果整理於下表1。 Then, the aluminum nitride fiber prepared in the specific example 1 and the comparative example 1 and the conventionally used aluminum nitride powder are respectively doped into the epoxy resin high score. Different test pieces were made in the sub-material, and thermal conductivity measurement was performed using a heat conduction analyzer, and the measured results were summarized in Table 1 below.
由表1所示之結果可知,利用添加本發明之氮化鋁纖維於高分子基材中,由於該些氮化鋁纖維可在高分子基材的內部建立良好的熱傳遞通路,因此,在較少添加量(40wt%)時即可與習知添加50wt%氮化鋁粉末的導熱性相當,而當本發明之氮化鋁纖維的添加量提升至50wt%時,其導熱性則可比添加相同含量的氮化鋁粉末提昇1.5倍。而由表1的試片2的結果得知,當添加氮化鋁纖維B-1於高分子基材時,其散熱性反而不佳,推測應是於製備氮化鋁纖維B-1的過程中,因為該氯化鋁溶液與氮化鋁粉末的比值過小,於煅燒過程產生的氧化物不足以包覆該等氮化鋁粉末,因此,不但無法有效形成氮化鋁纖維,反而會因為形成團聚物,無法有效散熱,而大幅的降低複合物的散熱效果。 It can be seen from the results shown in Table 1 that by adding the aluminum nitride fiber of the present invention to the polymer substrate, since the aluminum nitride fibers can establish a good heat transfer path inside the polymer substrate, The amount of addition (40 wt%) can be equivalent to the thermal conductivity of a conventionally added 50 wt% aluminum nitride powder, and when the amount of the aluminum nitride fiber of the present invention is increased to 50 wt%, the thermal conductivity is comparable. The same amount of aluminum nitride powder was increased by 1.5 times. From the results of the test piece 2 of Table 1, it is found that when the aluminum nitride fiber B-1 is added to the polymer substrate, the heat dissipation property is not good, and it is presumed that the process of preparing the aluminum nitride fiber B-1 should be performed. Because the ratio of the aluminum chloride solution to the aluminum nitride powder is too small, the oxide generated during the calcination process is insufficient to coat the aluminum nitride powder, so that not only the aluminum nitride fiber can be effectively formed, but also the formation The agglomerate cannot effectively dissipate heat, and greatly reduces the heat dissipation effect of the composite.
綜上所述,本發明利用電紡法製備高分子複合纖維,之後再利用煅燒方式將高分子材料移除即可得到氮化鋁纖維,而利用添加該氮化鋁纖維於高分子基材中,由於該些氮化鋁纖維可在高分子基材的內部建立良好的熱傳 遞通路,所以在較少添加量時即可具有相當的導熱性,由於可改善一般在高分子基材添加大量的氮化鋁粉體填充劑的做法,不僅可減低成本,而且也可避免添加過量的添充劑影響高分子基材基本物性的缺點,故確實能達成本發明之目的。 In summary, the present invention uses the electrospinning method to prepare a polymer composite fiber, and then removes the polymer material by calcination to obtain an aluminum nitride fiber, and the aluminum nitride fiber is added to the polymer substrate. Because these aluminum nitride fibers can establish good heat transfer inside the polymer substrate The transfer path has a relatively high thermal conductivity when added in a small amount, and the addition of a large amount of aluminum nitride powder filler generally on the polymer substrate can be improved, thereby not only reducing the cost but also avoiding the addition. Excessive additives affect the basic physical properties of the polymer substrate, so the object of the present invention can be achieved.
惟以上所述者,僅為本發明之較佳實施例而已,當不能以此限定本發明實施之範圍,即大凡依本發明申請專利範圍及專利說明書內容所作之簡單的等效變化與修飾,皆仍屬本發明專利涵蓋之範圍內。 The above is only the preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, that is, the simple equivalent changes and modifications made by the patent application scope and patent specification content of the present invention, All remain within the scope of the invention patent.
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CN106032586A (en) * | 2015-10-30 | 2016-10-19 | 大连交通大学 | Preparation method of high-orientation degree titanate fiber material |
CN111153685A (en) * | 2020-01-06 | 2020-05-15 | 佛山科学技术学院 | Continuous aluminum nitride fiber and preparation method thereof |
CN111188105A (en) * | 2020-01-15 | 2020-05-22 | 中国科学院化学研究所 | Aluminum nitride continuous nanofiber and preparation method thereof |
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CN106032586A (en) * | 2015-10-30 | 2016-10-19 | 大连交通大学 | Preparation method of high-orientation degree titanate fiber material |
CN106032586B (en) * | 2015-10-30 | 2018-06-01 | 大连交通大学 | A kind of preparation method of high-orientation titanate fibrous material |
CN111153685A (en) * | 2020-01-06 | 2020-05-15 | 佛山科学技术学院 | Continuous aluminum nitride fiber and preparation method thereof |
CN111188105A (en) * | 2020-01-15 | 2020-05-22 | 中国科学院化学研究所 | Aluminum nitride continuous nanofiber and preparation method thereof |
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