TW201904866A - Method for forming uniform carbon nanotube conductive paste and processing apparatus applied by the same wherein the conductive paste is provided with very stable physical properties and chemical properties - Google Patents

Method for forming uniform carbon nanotube conductive paste and processing apparatus applied by the same wherein the conductive paste is provided with very stable physical properties and chemical properties

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TW201904866A
TW201904866A TW106120968A TW106120968A TW201904866A TW 201904866 A TW201904866 A TW 201904866A TW 106120968 A TW106120968 A TW 106120968A TW 106120968 A TW106120968 A TW 106120968A TW 201904866 A TW201904866 A TW 201904866A
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conductive paste
agitator
carbon nanotube
planetary
forming
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TW106120968A
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Chinese (zh)
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TWI680943B (en
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賴鴻政
李依霖
梁家雄
林正崧
張曾隆
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識驊科技股份有限公司
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

Disclosed are a method for forming a uniform carbon nanotube conductive paste and a processing apparatus applied by the method. The method includes the following steps: applying a dispersant and NMP (N-methyl-2-pyrrolidone) to a planetary mixer, and performing a mixing and stirring operation; then adding a medium carbon nanotube to the planetary mixer, and continuously performing the mixing and stirring operation, wherein the medium carbon nanotube has a length of 5m to 10m and a diameter of 10 nm to 12 nm; then sequentially adding graphene and conductive carbon spheres (such as Super P) to the planetary agitator, so as to form a conductive paste; then feeding the conductive paste to a stirring and grinding mechanism, wherein the stirring and grinding mechanism includes another planetary mixer and a wet grinder connected in series with the another planetary mixer; pouring the conductive paste in the another planetary mixer and then circulating the conductive paste between the another planetary mixer and the wet grinder by a circulating conveyor mechanism. In this way, the medium carbon nanotube does not form an aggregate structure in the conductive paste so as to be effectively dispersed in the conductive paste, and the conductive paste as a whole forms a uniform structure, such that its physical properties and chemical properties may be very stable.

Description

形成均勻之奈米碳管導電漿料的方法及所應用之製程裝置  Method for forming uniform carbon nanotube conductive paste and applied process device  

本發明係有關於奈米碳管導電漿料之製造,尤其是一種形成均勻之奈米碳管導電漿料的方法及所應用之製程裝置。 The invention relates to the manufacture of a carbon nanotube conductive paste, in particular to a method for forming a uniform carbon nanotube conductive paste and a process device applied thereto.

電池主要是由正極及負極置於電解液中所形成。其中正極是將為數眾多的正極導電單元(正極材,如鈷酸鋰)混拌分散於漿料中。一般而言正極導電單元必須先與導電漿料混拌後方能應用於電極片上,並組裝成電池。因此眾多的正極導電單元(正極材)其彼此間是透過導電漿料所連接,因此導電漿料必須具有助導性或是導電性,方能使自由電子能在不同的正極導電單元中遷移且不必因內電阻而消耗過多能量,而達到有效之導電目的。因此製造漿料時必須考慮到使用特定導電材調節漿料之導電性。 The battery is mainly formed by placing a positive electrode and a negative electrode in an electrolyte. The positive electrode is a mixture of a plurality of positive electrode conductive units (positive electrode materials such as lithium cobalt oxide) dispersed in the slurry. In general, the positive conductive unit must be mixed with the conductive paste before it can be applied to the electrode sheets and assembled into a battery. Therefore, a plurality of positive electrode conductive units (positive electrode materials) are connected to each other through a conductive paste, and therefore the conductive paste must have conductivity or conductivity so that free electrons can migrate in different positive electrode conductive units. It is not necessary to consume too much energy due to internal resistance to achieve an effective conductive purpose. Therefore, it is necessary to adjust the conductivity of the slurry using a specific conductive material when manufacturing the slurry.

自從奈米碳管被開發以來,人類即發現奈米碳管為一種功能極為強大的材料,在機械工程、物理能源及生物科技上也大量地使用,達到許多實用上的目的。習知技術中已有使 用奈米碳管作為正極之導電漿料。 Since the development of the carbon nanotubes, humans have discovered that carbon nanotubes are extremely powerful materials, and they are also widely used in mechanical engineering, physical energy and biotechnology, achieving many practical purposes. A conductive paste using a carbon nanotube as a positive electrode has been known in the prior art.

在習知技術中型奈米碳管漿料之製作多使用單一長度或是管徑之奈米碳管。在長度與管徑上為單一平均數值,且其長度多以1~5μm之碳管製作,且純度亦是一大須克服之問題點。以短奈米碳管製作之正極漿料,理論上較無法像長碳一樣能跨越較多個正極導電單元,因此自由電子需跨越較多個導電係數差異介面使得因電阻所消耗之能量較多而影響正極極片之內電阻,降低電池表現。 In the prior art, a medium-sized carbon nanotube slurry is produced by using a single-length or diameter-diameter carbon nanotube. It is a single average value in length and diameter, and its length is more than 1~5μm carbon tube. The purity is also a major problem to be overcome. The positive electrode slurry made of short carbon nanotubes is theoretically less able to span more than one positive conductive unit like long carbon, so free electrons need to span more than one conductivity difference interface to make more energy due to resistance. It affects the internal resistance of the positive pole piece and reduces the battery performance.

有鑑於上述議題,本案發明人基於長久對於奈米碳管的研究及開發,發明人之研發團隊具備奈米碳管之生長技術,已將奈米碳管的相關技術多方利用於觸控面板、生醫敷材與功能性紡織,而這些研發成果也得到了相對應的專利亦或是申請中專利,如專利CN1483668A。在所知的範圍內,已將奈米碳管結合其於奈米材或是不同物性之奈米碳管應用在正極導電漿料中。因此發明人團隊在理解其奈米碳管材料優勢後將含不同形式的奈米碳管之奈米碳管漿料應用在正極之導電漿料。惟奈米碳管漿料在製程上尚有相當多的問題必須突破。 In view of the above issues, the inventor of the present invention based on the long-term research and development of carbon nanotubes, the inventor's research and development team has the growth technology of carbon nanotubes, and has applied various technologies related to carbon nanotubes to touch panels. Biomedical materials and functional textiles, and these research and development results have also received corresponding patents or application patents, such as the patent CN1483668A. Within the scope of the known, carbon nanotubes have been used in combination with nanomaterials or carbon nanotubes of different physical properties in the positive conducting paste. Therefore, the inventor team applied the carbon nanotube slurry containing different forms of carbon nanotubes to the conductive paste of the positive electrode after understanding the advantages of the carbon nanotube material. However, there are still quite a few problems in the process of nanocarbon tube slurry that must be broken.

發明人主要的貢獻是應用長度較長的奈米碳管於導電漿料中。一般奈米碳管本身為高分子聚合物且奈米碳管上的苯環彼此之間又有凡得瓦爾力,所以會聚集成團塊的結構,而 沉澱到溶液的底部,使整體導電漿料的導電性無法發揮。尤其是當奈米碳管的長度越長,直徑越小時,此種問題愈形嚴重。因此必須有有效的方法將團狀的奈米碳管分散,而且均勻分布到整個導電漿料區域,才能產生有效的作用。 The main contribution of the inventors is to apply a long length of carbon nanotubes in the conductive paste. Generally, the carbon nanotubes themselves are high molecular polymers and the benzene rings on the carbon nanotubes have a van der Waals force, so they are aggregated into a mass structure and precipitated to the bottom of the solution to make the overall conductive paste. The conductivity cannot be exerted. Especially when the length of the carbon nanotube is longer and the diameter is smaller, the problem becomes more serious. Therefore, an effective method must be used to disperse the agglomerated carbon nanotubes and evenly distribute them throughout the conductive paste region to produce an effective effect.

故本案希望提出一種嶄新的形成均勻之奈米碳管導電漿料的方法及所應用之製程裝置,以解決上述先前技術上的缺陷。 Therefore, the present invention intends to propose a new method for forming a uniform carbon nanotube conductive paste and a processing device applied thereto to solve the above-mentioned prior art defects.

所以本發明的目的係為解決上述習知技術上的問題,本發明中提出一種形成均勻之奈米碳管導電漿料的方法及所應用之製程裝置,係應用行星式攪拌器將中型奈米碳管與分散劑、導電碳球及NMP混合形成導電漿料。該行星式攪拌器中的公轉式攪拌器,用於將該導電漿料作大路徑的攪拌,以使得該導電漿料在該內桶內部形成較大區域的位移。該行星式攪拌器中的自轉式攪拌器係用於將該導電漿料作做局部的充分攪拌,主要是由塊狀體沿著自身的軸線作自轉,而使得在該自轉式攪拌器周圍的該導電漿料形成渦流。當漿料從行星式攪拌器傳送至一溼式研磨機後,經由溼式研磨機的研磨珠體會撞擊內部的導電漿料而將該導電漿料中的奈米碳管充分打散,原來團聚在一起的奈米碳管,會因為該研磨珠體的撞擊而被打散。且經過該行星式攪拌器及該溼式研磨機來回攪 拌撞擊,一方面使得中型奈米碳管不會形成聚集的結構,有效的分散在該導電漿料中,而且整體導電漿料形成均勻的結構,所以其物性及化性可以相當的均勻。 Therefore, the object of the present invention is to solve the above-mentioned problems in the prior art. In the present invention, a method for forming a uniform carbon nanotube conductive paste and a process device therefor are proposed, which are to apply a planetary agitator to a medium-sized nanometer. The carbon tube is mixed with a dispersant, a conductive carbon ball, and NMP to form a conductive paste. The revolving agitator in the planetary agitator is used for agitating the conductive slurry in a large path so that the conductive slurry forms a large area displacement inside the inner tub. The self-rotating agitator in the planetary agitator is used for partially stirring the conductive slurry, mainly by rotating the block body along its own axis, so as to be around the self-rotating agitator. The conductive paste forms a vortex. After the slurry is transferred from the planetary agitator to a wet mill, the grinding beads passing through the wet mill will strike the inner conductive slurry to fully dissipate the carbon nanotubes in the conductive slurry, and the original agglomeration The carbon nanotubes together will be broken up due to the impact of the grinding beads. And the planetary stirrer and the wet grinder repeatedly agitate and impact, on the one hand, the medium-sized carbon nanotubes do not form an aggregate structure, are effectively dispersed in the conductive paste, and the overall conductive paste is formed uniformly. Structure, so its physical properties and chemical properties can be fairly uniform.

為達到上述目的本發明中提出一種形成均勻之奈米碳管導電漿料的方法,包含下列步驟:第一製程為預混拌製程,包含步驟為:步驟A:將分散劑與NMP(N-Methyl-2-pyrrolidone,N-甲基吡咯烷酮)加入一第一行星式攪拌器中,並進行混合及攪拌的作業;其中該NMP係作為溶劑之用;步驟B:然後將中型奈米碳管加入該第一行星式攪拌器中繼續進行混合及攪拌的作業;其中該中型奈米碳管的長度介於5μm到10μm之間,而直徑為10nm到12nm之間;步驟C:然後將石墨烯(graphene)加入該第一行星式攪拌器中繼續進行混合及攪拌的作業;步驟D:然後將導電碳球(如Super P)加入該第一行星式攪拌器中繼續進行混合及攪拌的作業;所以該第一行星式攪拌器的該內桶內的該分散劑、該NMP、該中型奈米碳管、該石墨烯及該導電碳球形成導電漿料;第二製程為研磨攪拌製程,包含步驟為:步驟E:將上述第一製程所混合及攪拌的該導電漿料饋送到一攪拌研磨機構,其中該攪拌研磨機構包含一第二行星式攪拌器及與該第二行星式攪拌器相串聯的一溼式研磨器;該導電漿料先灌注入該第二行星式攪拌器之後由循環傳送機構讓該導電漿料在該第二行星式攪拌器及該 溼式研磨器之間循環流動;該導電漿料在該第二行星式攪拌器及該溼式研磨器之間來回流動。 In order to achieve the above object, a method for forming a uniform carbon nanotube conductive paste is provided, which comprises the following steps: the first process is a premixing process, and the steps include: Step A: dispersing agent and NMP (N- Methyl-2-pyrrolidone, N-methylpyrrolidone) is added to a first planetary agitator and mixed and stirred; wherein the NMP is used as a solvent; Step B: then the medium carbon nanotube is added The mixing and stirring operation is continued in the first planetary agitator; wherein the medium-sized carbon nanotube has a length between 5 μm and 10 μm and a diameter between 10 nm and 12 nm; and step C: then graphene ( Graphene) adding the first planetary agitator to continue the mixing and stirring operation; step D: then adding a conductive carbon ball (such as Super P) to the first planetary agitator to continue the mixing and stirring operation; The dispersing agent, the NMP, the medium-sized carbon nanotube, the graphene and the conductive carbon ball in the inner barrel of the first planetary agitator form a conductive paste; the second process is a grinding and agitating process, including the steps For: step E: feeding the conductive paste mixed and stirred in the first process to a stirring grinding mechanism, wherein the stirring grinding mechanism comprises a second planetary agitator and a wetness in series with the second planetary agitator a grinder; the conductive paste is first poured into the second planetary agitator, and the conductive slurry is circulated between the second planetary agitator and the wet grinder by a circulation conveying mechanism; the conductive paste The material flows back and forth between the second planetary agitator and the wet grinder.

本案尚提出一種形成均勻之奈米碳管導電漿料的攪拌研磨機構,係將一行星式攪拌器串聯一溼式研磨器,其中該導電漿料先灌注入該行星式攪拌器之後由循環傳送機構讓該導電漿料在該行星式攪拌器及該溼式研磨器之間循環流動;該導電漿料在該行星式攪拌器及該溼式研磨器之間來回流動,應用不同的攪拌及撞擊方式以達到該導電漿料中的奈米碳管的充分分散的效用;其中該導電漿料先在該第二行星式攪拌器適當的攪拌後,再送入該溼式研磨器,由於該珠磨攪拌器的轉動,該溼式研磨器內的研磨珠體撞擊內部的該導電漿料而將該導電漿料中的奈米碳管充分打散,原來團聚在一起的奈米碳管,因為該研磨珠體的撞擊而被打散;該導電漿料必須在該行星式攪拌器及該溼式研磨器之間來回流動,應用不同的攪拌及撞擊方式以達到該導電漿料中的奈米碳管的充分分散的效用。 In this case, a stirring and grinding mechanism for forming a uniform conductive carbon nanotube conductive slurry is proposed, in which a planetary agitator is connected in series with a wet grinder, wherein the conductive paste is firstly poured into the planetary agitator and then transferred by circulation. The mechanism circulates the conductive paste between the planetary agitator and the wet grinder; the conductive paste flows back and forth between the planetary agitator and the wet grinder, applying different agitation and impact In order to achieve the effect of sufficient dispersion of the carbon nanotubes in the electrically conductive paste; wherein the electrically conductive paste is first fed to the wet grinder after proper agitation of the second planetary agitator, due to the bead mill Rotating the agitator, the grinding bead in the wet grinder hits the inner conductive paste to fully dissipate the carbon nanotubes in the conductive paste, and the carbon nanotubes originally reunited together because The impact of the bead is broken up; the conductive paste must flow back and forth between the planetary agitator and the wet grinder, and different agitation and impact modes are applied to achieve the nanocarbon in the conductive paste. tube Fully dispersed effectiveness.

由下文的說明可更進一步瞭解本發明的特徵及其優點,閱讀時並請參考附圖。 The features of the present invention and its advantages are further understood from the following description, and reference is made to the accompanying drawings.

1‧‧‧攪拌研磨機構 1‧‧‧Agitating grinding mechanism

10‧‧‧行星式攪拌器 10‧‧‧ planetary mixer

11‧‧‧內桶 11‧‧‧ inner barrel

12‧‧‧外桶 12‧‧‧ outer barrel

20‧‧‧公轉式攪拌器 20‧‧‧Rotary agitator

25‧‧‧框架 25‧‧‧Frame

30‧‧‧自轉式攪拌器 30‧‧‧Rotary agitator

35‧‧‧轉球 35‧‧‧ Turn the ball

40‧‧‧溼式研磨器 40‧‧‧Wet grinder

41‧‧‧研磨桶 41‧‧‧ grinding bucket

42‧‧‧過濾器 42‧‧‧Filter

50‧‧‧珠磨攪拌器 50‧‧‧Bead mill mixer

60‧‧‧研磨珠體 60‧‧‧ grinding beads

70‧‧‧循環傳送機構 70‧‧‧Circular transmission mechanism

100‧‧‧冷卻水 100‧‧‧cooling water

101‧‧‧第一行星式攪拌器 101‧‧‧First planetary agitator

102‧‧‧第二行星式攪拌器 102‧‧‧Second planetary agitator

201‧‧‧驅動機構 201‧‧‧ drive mechanism

202‧‧‧驅動機構 202‧‧‧ drive mechanism

203‧‧‧驅動機構 203‧‧‧ drive mechanism

251‧‧‧刀片 251‧‧‧blade

351‧‧‧懸鐵柱 351‧‧‧ hanging iron column

圖1顯示本案之行星式攪拌器之示意圖。 Figure 1 shows a schematic view of the planetary agitator of the present case.

圖2顯示本案之溼式研磨器之示意圖。 Figure 2 shows a schematic view of the wet grinder of the present invention.

圖3顯示本案之攪拌研磨機構之示意圖。 Figure 3 shows a schematic view of the agitating and grinding mechanism of the present invention.

圖4顯示本案之第一行星式攪拌器、第二行星式攪拌器 及溼式研磨器之連接示意圖。 Fig. 4 is a view showing the connection of the first planetary agitator, the second planetary agitator and the wet grinder of the present invention.

圖5顯示本案之方法步驟流程圖。 Figure 5 shows a flow chart of the method steps of the present case.

茲謹就本案的結構組成,及所能產生的功效與優點,配合圖式,舉本案之一較佳實施例詳細說明如下。 In view of the structural composition of the case, and the functions and advantages that can be produced, in conjunction with the drawings, a preferred embodiment of the present invention is described in detail below.

請參考圖1至圖4所示,顯示本發明之形成均勻之奈米碳管導電漿料的方法及所應用之製程裝置,包含下列元件:一行星式攪拌器10,主要是用於攪拌導電漿料,讓該導電漿料內的各個成分可以均勻混合,尤其是可以將奈米碳管與分散劑充分混合,不會使奈米碳管聚積成塊狀結構。 Referring to FIG. 1 to FIG. 4, a method for forming a uniform carbon nanotube conductive paste of the present invention and a processing device therefor are provided, comprising the following components: a planetary agitator 10, mainly for stirring and conducting electricity. The slurry allows the components in the conductive paste to be uniformly mixed. In particular, the carbon nanotubes can be thoroughly mixed with the dispersing agent without accumulating the carbon nanotubes into a massive structure.

如圖1所示,該行星式攪拌器10主要包含:一內桶11,用於放置該導電漿料,並攪拌該導電漿料。 As shown in FIG. 1, the planetary agitator 10 mainly comprises an inner tub 11 for placing the conductive paste and agitating the conductive paste.

一外桶12,係容納該內桶11,該外桶12及該內桶11之間配置有冷卻水100,以冷卻該內桶11內部的該導電漿料,冷卻水100可外接循環冷卻系統(為熟知之習知技術,不贅述其細部結構),以達到冷卻水100循環及熱交換的效果。 An outer tub 12 is disposed to receive the inner tub 11 . The outer tub 12 and the inner tub 11 are disposed with cooling water 100 to cool the conductive paste inside the inner tub 11 , and the cooling water 100 can be externally connected to the circulating cooling system. (For well-known conventional techniques, the detailed structure is not described in detail) to achieve the effect of 100 cycles of cooling water and heat exchange.

一公轉式攪拌器20,配置於該內桶11內,並外接驅動機構201,該公轉式攪拌器20係用於將該導電漿料作大路徑的攪拌,以使得該導電漿料在該內桶11內部形成較大區域的位移。其中該公轉式攪拌器20為一近似U形或V形的框架25,並在該框架25的側邊配置多數個刀片251的結構。攪拌時該公轉式攪拌器20沿著該框架25的軸線轉動,而使得該導電漿料形成較大路徑的位移。較佳者該公轉式攪拌器20轉動時所掃出的體積超過該內桶11容積之一半。 a slewing agitator 20 disposed in the inner tub 11 and externally connected to the driving mechanism 201 for agitating the conductive slurry in a large path so that the conductive paste is inside The inside of the tub 11 forms a displacement of a large area. The revolving agitator 20 is an approximately U-shaped or V-shaped frame 25, and a plurality of blades 251 are disposed on the side of the frame 25. The agitating agitator 20 rotates along the axis of the frame 25 while agitating, causing the conductive paste to form a displacement of a larger path. Preferably, the volume swept out by the revolutionary agitator 20 exceeds one half of the volume of the inner tub 11.

一自轉式攪拌器30,係用於將該導電漿料做局部的充分攪拌,主要是由塊狀體沿著自身的軸線作自轉,而使得在該自轉式攪拌器30周圍的該導電漿料形成渦流。本案中該自轉式攪拌器30為一轉球35,並由一懸鐵柱351懸吊,再經由驅動機構202加以驅動。轉動時該轉球35繞著通過其球心的軸線轉動,而對該導電漿料形成渦流。 A self-rotating agitator 30 is used for partially agitating the conductive paste, mainly by rotating the block body along its own axis, so that the conductive paste around the rotary agitator 30 Forming eddy currents. In the present case, the rotary agitator 30 is a ball 35 and is suspended by a suspension column 351 and driven by a drive mechanism 202. When rotated, the ball 35 rotates about the axis passing through its center of the ball to form a vortex to the conductive paste.

本案中該自轉式攪拌器30所配置的轉球35可為多個,各個轉球35分別經由一懸鐵柱351懸吊,各個轉球35的旋轉方向可相同或不同。在圖中以兩個轉球35作為說明。 In the present case, the rotary agitator 30 may be provided with a plurality of rotating balls 35, and each of the rotating balls 35 is suspended by a suspension column 351, and the rotation directions of the respective rotating balls 35 may be the same or different. In the figure, two turning balls 35 are taken as an illustration.

本案中自轉的目的在於使得該導電漿料形成局部性的渦流,主要是將團聚的奈米碳管打散。公轉的目的在於使得該內桶11的該導電漿料形成大位移的對流,而使得整體該導電漿料可以均勻分布。所以利用公轉及自轉充分的將該導電漿料完全融合。 The purpose of the rotation in this case is to cause the conductive paste to form a local eddy current, mainly to break up the agglomerated carbon nanotubes. The purpose of the revolution is to cause the conductive paste of the inner tub 11 to form a large displacement convection, so that the entire conductive paste can be uniformly distributed. Therefore, the conductive paste is fully fused by revolution and rotation.

一溼式研磨器40,如圖2所示,包含:一研磨桶41,該研磨桶41內配置有該導電漿料。 A wet grinder 40, as shown in FIG. 2, comprises: a grinding barrel 41 in which the conductive paste is disposed.

一珠磨攪拌器50,係配置在該研磨桶41內部,用於將該導電漿料充分的攪拌。 A bead mill agitator 50 is disposed inside the grinding tub 41 for sufficiently agitating the conductive paste.

多數個研磨珠體60,配置在該研磨桶41內部,當珠磨攪拌器50攪拌時,該研磨珠體60會撞擊內部的該導電漿料而將該導電漿料中的奈米碳管充分打散,原來團聚在一起的奈米碳管,會因為該研磨珠體60的撞擊而被打散。較佳者該研磨珠體60的尺寸介於0.5mm到1.3mm之間,且該研磨珠體60以氧化鋯製作而成。 A plurality of grinding beads 60 are disposed inside the grinding drum 41. When the bead mill mixer 50 is agitated, the grinding beads 60 may impinge on the inner conductive paste to sufficiently fill the carbon nanotubes in the conductive paste. Breaking up, the carbon nanotubes that were originally reunited together will be broken up due to the impact of the grinding beads 60. Preferably, the size of the bead body 60 is between 0.5 mm and 1.3 mm, and the bead body 60 is made of zirconia.

一過濾器42,用於將該研磨桶41中的該導電漿料過濾後得到均勻的該導電漿料再往外輸送。本案中該過濾器42係配置在該研磨桶41的前端,將 該導電漿料擠壓過該過濾器42後再由該研磨桶41的一端往外傳送。 A filter 42 is configured to filter the conductive paste in the grinding drum 41 to obtain a uniform conductive slurry for further transportation. In the present case, the filter 42 is disposed at the front end of the grinding tub 41, and the conductive paste is extruded through the filter 42 and then conveyed outward from one end of the grinding tub 41.

如圖3所示,本案中用於形成均勻之奈米碳管導電漿料的攪拌研磨機構1係將該行星式攪拌器10串聯該溼式研磨器40,該導電漿料先灌注入該行星式攪拌器10之後由循環傳送機構70讓該導電漿料在該行星式攪拌器10及該溼式研磨器40之間循環流動。一般該行星式攪拌器10的容積遠大於該溼式研磨器40的容積,該導電漿料必須在該行星式攪拌器10及該溼式研磨器40之間來回流動,應用不同的攪拌及撞擊方式以達到該導電漿料中的奈米碳管的充分分散的效用。該循環傳送機構70可經由一驅動機構203驅動。該循環傳送機構70為一般所熟知之機構,所以在文中並不說明其細部,圖式所顯示者僅為示意圖。 As shown in FIG. 3, in the present embodiment, the agitating and grinding mechanism 1 for forming a uniform carbon nanotube conductive paste is in which the planetary agitator 10 is connected in series to the wet grinder 40, and the conductive paste is first poured into the planet. The agitator 10 is then circulated by the circulation transfer mechanism 70 between the planetary agitator 10 and the wet grinder 40. Generally, the volume of the planetary agitator 10 is much larger than the volume of the wet grinder 40. The conductive paste must flow back and forth between the planetary agitator 10 and the wet grinder 40, applying different agitation and impact. The method is to achieve the effect of sufficient dispersion of the carbon nanotubes in the conductive paste. The circulation transfer mechanism 70 can be driven via a drive mechanism 203. The recirculating mechanism 70 is a generally well-known mechanism, so its details are not described herein, and the figures are only schematic.

如圖5所示,本案中形成均勻之奈米碳管導電漿料的方法步驟說明如下: As shown in FIG. 5, the method steps for forming a uniform carbon nanotube conductive paste in the present case are as follows:

第一製程為預混拌製程:將分散劑與NMP(N-Methyl-2-pyrrolidone,N-甲基吡咯烷酮)加入一第一行星式攪拌器101中(如圖4所示),並進行混合及攪拌的作業(步驟801),其時間約15到20分鐘。其中該NMP係作為溶劑之用。其中該第一行星式攪拌器101的結構同於上述之行星式攪拌器10。 The first process is a pre-mixing process: adding a dispersant and NMP (N-Methyl-2-pyrrolidone, N-methylpyrrolidone) to a first planetary agitator 101 (as shown in FIG. 4) and mixing And the agitating operation (step 801), the time is about 15 to 20 minutes. Among them, the NMP is used as a solvent. The structure of the first planetary agitator 101 is the same as that of the planetary agitator 10 described above.

其中該第一行星式攪拌器101的該公轉式攪拌器20的公轉頻率為40rpm(rotation per minute),該第一行星式攪拌器101的該自轉式攪拌器30為兩顆轉球35,其自轉頻率為200rpm,兩顆轉球35為同向旋轉。 The revolution frequency of the revolutionary agitator 20 of the first planetary agitator 101 is 40 rpm (rotation per minute), and the rotary agitator 30 of the first planetary agitator 101 is two rotating balls 35. The rotation frequency is 200 rpm, and the two balls 35 rotate in the same direction.

然後將中型奈米碳管加入該第一行星式攪拌器101中繼續進行混合及攪拌的作業(步驟802),其時間約30到60分鐘,其中該第一行星式攪拌器101的該公轉式攪拌器20的公轉頻率為40rpm,該第一行星式攪拌器101的該自轉式攪拌器30為兩顆轉球35,其自轉頻率為1200rpm,兩顆轉球35為反向旋轉。 The medium carbon nanotube is then added to the first planetary agitator 101 to continue the mixing and agitation operation (step 802) for a period of about 30 to 60 minutes, wherein the revolution of the first planetary agitator 101 The revolving frequency of the agitator 20 is 40 rpm, and the autorotating agitator 30 of the first planetary agitator 101 is two rotating balls 35 having a rotation frequency of 1200 rpm, and the two rotating balls 35 are reversely rotated.

然後將石墨烯(graphene)加入該第一行星式攪拌器101中繼續進行混合及攪拌的作業(步驟803),其時間約30到60分鐘,其中該第一行星式攪拌器101的該公轉式攪拌器20的公轉頻率為40rpm,該第一行星式攪拌器101的該自轉式攪拌器30為兩顆轉球35,其自轉頻率為800rpm,兩顆轉球35為反向旋轉。 Graphene is then added to the first planetary agitator 101 to continue the mixing and agitation operation (step 803) for a period of about 30 to 60 minutes, wherein the revolution of the first planetary agitator 101 The revolving frequency of the agitator 20 is 40 rpm, and the autorotating agitator 30 of the first planetary agitator 101 is two rotating balls 35 having a rotation frequency of 800 rpm, and the two rotating balls 35 are reversely rotated.

然後將導電碳球(如Super P)加入該第一行星式攪拌器101中繼續進行混合及攪拌的作業,其時間約30到40分鐘。所以該第一行星式攪拌器101的該內桶11內的該分散劑、該NMP、該中型奈米碳管、該石墨烯及該導電碳球形成導電漿料(步驟804)。其中該第一行星式攪拌器101的該公轉式攪拌 器20的公轉頻率為40rpm,該第一行星式攪拌器101的該自轉式攪拌器30為兩顆轉球35,其自轉頻率為600rpm,兩顆轉球35為反向旋轉。 A conductive carbon ball (e.g., Super P) is then added to the first planetary agitator 101 to continue the mixing and agitation operation for about 30 to 40 minutes. Therefore, the dispersant, the NMP, the medium-sized carbon nanotube, the graphene and the conductive carbon ball in the inner tub 11 of the first planetary agitator 101 form a conductive paste (step 804). The revolution frequency of the revolutionary agitator 20 of the first planetary agitator 101 is 40 rpm, and the rotation agitator 30 of the first planetary agitator 101 is two rotating balls 35, and the rotation frequency thereof is 600 rpm. The two balls 35 are reversely rotated.

上述第一製程中的各步驟作用的溫度在20到30℃之間。 The temperature at each step in the first process described above is between 20 and 30 °C.

其中該分散劑佔整個導電漿料的比例約在0.8%~1.2%重量百分比之間;該分散劑主要用於將該中型奈米碳管撐開,而不會聚集成一團,甚或下沉到底部,而使得該中型奈米碳管可以在該導電漿料中呈均勻的分布。該分散劑可包含高分子分散劑及低分子分散劑。其中該高分子分散劑與低分子分散劑的比例為7:3。 Wherein the dispersant accounts for about 0.8% to 1.2% by weight of the entire conductive paste; the dispersant is mainly used to open the medium-sized carbon nanotubes without being aggregated, or even sinking to the end. And the medium-sized carbon nanotubes can be uniformly distributed in the conductive paste. The dispersant may comprise a polymeric dispersant and a low molecular dispersant. The ratio of the polymer dispersant to the low molecular dispersant is 7:3.

其中該高分子分散劑如PVP(Polyvinylpyrrolidone,聚乙烯吡咯烷酮)。其中低分子分散劑如苯磺酸鹽類、溴化銨鹽類及采酮(TritonX-100);該苯磺酸鹽類為任一種苯磺酸鹽類均可達到本案的效果;其中該溴化銨鹽類可以如CTAB(cetyltrimethylammonium bromide,溴化十六烷基三甲銨)。其中PVP、苯磺酸鹽類、溴化銨鹽類及采酮的比例為7:2:0.5:0.5。 The polymer dispersant is, for example, PVP (Polyvinylpyrrolidone, polyvinylpyrrolidone). Among them, low molecular dispersants such as besylate, ammonium bromide and ketene (Triton X-100); the besylate can be any of the besylate salts; The ammonium salts may be, for example, CTAB (cetyltrimethylammonium bromide, cetyltrimethylammonium bromide). The ratio of PVP, besylate, ammonium bromide and ketene is 7:2:0.5:0.5.

其中該中型奈米碳管佔整個該導電漿料的比例約在1%~5%重量百分比之間;其中該中型奈米碳管的長度介於5μm到10μm之間,而直徑約為10nm到12nm之間。 Wherein the medium-sized carbon nanotubes account for about 1% to 5% by weight of the entire conductive paste; wherein the medium-sized carbon nanotubes have a length of between 5 μm and 10 μm, and the diameter is about 10 nm. Between 12nm.

其中該石墨烯佔整個該導電漿料的比例約在0.2%~1.2%重量百分比之間;該石墨烯包含兩種型態,一種為具有二至四層之結構的石墨烯,其佔整個該導電漿料的比例大於0%重量百分比;另一種則為具有四至八層之結構的石墨烯,其佔整個該導電漿料的比例大於0%重量百分比,兩種的組合佔整個該導電漿料的比例約在0.2%~1.2%重量百分比之間。 Wherein the ratio of the graphene to the entire conductive paste is between about 0.2% and 1.2% by weight; the graphene comprises two types, one is graphene having a structure of two to four layers, which accounts for the whole The ratio of the conductive paste is greater than 0% by weight; the other is graphene having a structure of four to eight layers, which accounts for more than 0% by weight of the entire conductive paste, and the combination of the two accounts for the entire conductive paste. The ratio is between about 0.2% and 1.2% by weight.

其中該導電碳球佔整個該導電漿料的比例約在0%~1.5%重量百分比之間。 The ratio of the conductive carbon sphere to the entire conductive paste is between about 0% and 1.5% by weight.

第二製程為研磨攪拌製程,係將上述第一製程所混合及攪拌的該導電漿料饋送到一攪拌研磨機構1(如圖4所示),該攪拌研磨機構1包含一第二行星式攪拌器102及相串聯的該溼式研磨器40。該導電漿料先灌注入該第二行星式攪拌器102之後由循環傳送機構70讓該導電漿料在該第二行星式攪拌器102及該溼式研磨器40之間循環流動(步驟805)。其中該第二行星式攪拌器102的結構同於上述之行星式攪拌器10。 The second process is a grinding and agitating process, and the conductive slurry mixed and stirred in the first process is fed to a stirring and grinding mechanism 1 (as shown in FIG. 4), and the agitating and grinding mechanism 1 includes a second planetary stirring. The device 102 and the wet grinder 40 are connected in series. After the conductive paste is first poured into the second planetary agitator 102, the conductive slurry is circulated between the second planetary agitator 102 and the wet grinder 40 by a circulation transfer mechanism 70 (step 805). . The structure of the second planetary agitator 102 is the same as that of the planetary agitator 10 described above.

其中該導電漿料先在該第二行星式攪拌器102適當的攪拌後,再送入該溼式研磨器40,由於該珠磨攪拌器50的轉動,該研磨珠體60會撞擊內部的該導電漿料而將該導電漿料中的中型奈米碳管充分打散,原來團聚在一起的奈米碳管,會因為該研磨珠體60的撞擊而被打散,經過充分的攪拌撞擊, 原來中型奈米碳管團聚在一起所形成的團聚體的直徑可到小於100μm。該導電漿料必須在該第二行星式攪拌器102及該溼式研磨器40之間來回流動,應用不同的攪拌及撞擊方式以達到該導電漿料中的奈米碳管的充分分散的效用。 The conductive paste is first sent to the wet grinder 40 after being properly stirred by the second planetary agitator 102. Due to the rotation of the bead mill agitator 50, the bead body 60 may impinge on the internal conductive. The medium-sized carbon nanotubes in the conductive slurry are sufficiently dispersed by the slurry, and the carbon nanotubes originally agglomerated together are broken up due to the impact of the grinding beads 60, and after sufficient agitation and impact, the original The agglomerates formed by the agglomeration of the medium carbon nanotubes may have a diameter of less than 100 μm. The conductive paste must flow back and forth between the second planetary agitator 102 and the wet grinder 40, and different agitation and impact modes are applied to achieve the full dispersion effect of the carbon nanotubes in the conductive paste. .

在本案中該珠磨攪拌器50的轉速為2000到3000rpm。操作溫度小於35℃。 In the present case, the bead mill agitator 50 has a rotational speed of 2000 to 3000 rpm. Operating temperature is less than 35 °C.

本案應用上述的兩個製程即可達到所需之均勻度。 In this case, the above two processes can be applied to achieve the required uniformity.

第三製程為儲料混拌製程,係將上述所得到的該導電漿料取出後,測量其黏度以決定該導電漿料是否符合所需要的黏度,然後再封裝以作為商品買賣之用。其中黏度的要求為在2rpm下黏度可以達到8000到12000cps(步驟806)。 The third process is a stock mixing process, after the conductive paste obtained above is taken out, the viscosity is measured to determine whether the conductive paste meets the required viscosity, and then packaged for sale as a commodity. The viscosity requirement is that the viscosity can reach 8000 to 12000 cps at 2 rpm (step 806).

本案中應用上述製程可以將中型奈米碳管與分散劑、導電碳球及NMP混合,該行星式攪拌器中的公轉式攪拌器,用於將該導電漿料作大路徑的攪拌,以使得該導電漿料在該內桶內部形成較大區域的位移。該行星式攪拌器中的自轉式攪拌器係用於將該導電漿料作做局部的充分攪拌,主要是由塊狀體沿著自身的軸線作自轉,而使得在該自轉式攪拌器周圍的該導電漿料形成渦流。該溼式研磨器的研磨珠體會撞擊內部的導電漿料而將該導電漿料中的奈米碳管充分打散,原來團聚在一起的奈米碳管,會因為該研磨珠體的撞擊而被打散。 In the present application, the medium-sized carbon nanotubes can be mixed with a dispersing agent, a conductive carbon ball and an NMP, and a revolving agitator in the planetary agitator is used for stirring the conductive slurry in a large path, so that The conductive paste forms a large area displacement inside the inner tub. The self-rotating agitator in the planetary agitator is used for partially stirring the conductive slurry, mainly by rotating the block body along its own axis, so as to be around the self-rotating agitator. The conductive paste forms a vortex. The grinding beads of the wet grinder collide with the inner conductive paste to fully dissipate the carbon nanotubes in the conductive paste, and the carbon nanotubes originally agglomerated together may be hit by the grinding beads. Was broken up.

經過該行星式攪拌器及該溼式研磨機來回攪拌撞擊,一方面使得中型奈米碳管不會形成聚集的結構,有效的分散在該導電漿料中,而且整體該導電漿料形成均勻的結構,所以其物性及化性可以相當的均勻。 After the planetary stirrer and the wet grinder are stirred back and forth, on the one hand, the medium-sized carbon nanotubes do not form an aggregate structure, are effectively dispersed in the conductive paste, and the conductive paste is uniformly formed as a whole. Structure, so its physical properties and chemical properties can be fairly uniform.

綜上所述,本案人性化之體貼設計,相當符合實際需求。其具體改進現有缺失,相較於習知技術明顯具有突破性之進步優點,確實具有功效之增進,且非易於達成。本案未曾公開或揭露於國內與國外之文獻與市場上,已符合專利法規定。 In summary, the humanized design of this case is quite in line with actual needs. The specific improvement of the existing defects is obviously a breakthrough improvement advantage compared with the prior art, and it has an improvement in efficacy and is not easy to achieve. The case has not been disclosed or disclosed in domestic and foreign literature and market, and has complied with the provisions of the Patent Law.

上列詳細說明係針對本發明之一可行實施例之具體說明,惟該實施例並非用以限制本發明之專利範圍,凡未脫離本發明技藝精神所為之等效實施或變更,均應包含於本案之專利範圍中。 The detailed description of the preferred embodiments of the present invention is intended to be limited to the scope of the invention, and is not intended to limit the scope of the invention. The patent scope of this case.

Claims (21)

一種形成均勻之奈米碳管導電漿料的方法,包含下列步驟:第一製程為預混拌製程,包含步驟為:步驟A:將分散劑與NMP(N-Methyl-2-pyrrolidone,N-甲基吡咯烷酮)加入一第一行星式攪拌器中,並進行混合及攪拌的作業;其中該NMP係作為溶劑之用;步驟B:然後將中型奈米碳管加入該第一行星式攪拌器中繼續進行混合及攪拌的作業;其中該中型奈米碳管的長度介於5μm到10μm之間,而直徑為10nm到12nm之間;步驟C:然後將石墨烯(graphene)加入該第一行星式攪拌器中繼續進行混合及攪拌的作業;步驟D:然後將導電碳球加入該第一行星式攪拌器中繼續進行混合及攪拌的作業;所以該第一行星式攪拌器的該內桶內的該分散劑、該NMP、該中型奈米碳管、該石墨烯及該導電碳球形成導電漿料;第二製程為研磨攪拌製程,包含步驟為:步驟E:將上述第一製程所混合及攪拌的該導電漿料饋送到一攪拌研磨機構,其中該攪拌研磨機構包含一第二行星式攪拌器及與該第二行星式攪拌器相串聯的一溼式研磨器;該導電漿料先灌注入該第二行星式攪拌器之後由循環傳送機構讓該導電漿料在該第二行星式攪拌器及該溼式研磨器之間 循環流動;該導電漿料在該第二行星式攪拌器及該溼式研磨器之間來回流動。  A method for forming a uniform carbon nanotube conductive paste comprises the following steps: the first process is a premixing process, and the steps are: Step A: dispersing agent and NMP (N-Methyl-2-pyrrolidone, N- Methylpyrrolidone) is added to a first planetary agitator and mixed and stirred; wherein the NMP is used as a solvent; Step B: a medium carbon nanotube is then added to the first planetary agitator The mixing and stirring operation is continued; wherein the medium carbon nanotube has a length between 5 μm and 10 μm and a diameter between 10 nm and 12 nm; and step C: then graphene is added to the first planetary Mixing and stirring are continued in the agitator; Step D: then adding conductive carbon balls to the first planetary agitator to continue mixing and stirring; therefore, the inside of the inner barrel of the first planetary agitator The dispersing agent, the NMP, the medium-sized carbon nanotube, the graphene and the conductive carbon ball form a conductive paste; the second process is a grinding and agitating process, and the steps include: Step E: mixing the first process and Stirring The conductive paste is fed to a stirring grinding mechanism, wherein the agitating grinding mechanism comprises a second planetary agitator and a wet grinder in series with the second planetary agitator; the conductive paste is first poured into the first After the two planetary agitators, the conductive slurry is circulated between the second planetary agitator and the wet grinder by a circulating conveying mechanism; the conductive slurry is in the second planetary agitator and the wet type The grinder flows back and forth between the grinders.   如申請專利範圍第1項所述之形成均勻之奈米碳管導電漿料的方法,其中該第一行星式攪拌器及該第二行星式攪拌器均包含:一內桶,用於放置導電漿料,並攪拌該導電漿料;一外桶,係容納該內桶,該外桶及該內桶之間配置有冷卻水,以冷卻該內桶內部的該導電漿料;一公轉式攪拌器,配置於該內桶內,並外接驅動機構,該公轉式攪拌器係用於將該導電漿料作大路徑的攪拌,以使得該導電漿料在該內桶內部形成較大區域的位移;該公轉式攪拌器為一近似U形或V形的框架,並在該框架的側邊配置多數個刀片的結構;一自轉式攪拌器,係用於將該導電漿料做局部的充分攪拌,主要是由塊狀體沿著自身的軸線作自轉,而使得在該自轉式攪拌器周圍的該導電漿料形成渦流;該自轉式攪拌器為二轉球,各該轉球分別由一懸鐵柱懸吊,再經由驅動機構加以驅動;轉動時各該轉球繞著通過其自身球心的軸線轉動,而對該導電漿料形成渦流。  The method for forming a uniform carbon nanotube conductive paste according to claim 1, wherein the first planetary agitator and the second planetary agitator each comprise: an inner barrel for placing conductive Slurry, and stirring the conductive slurry; an outer tub is for accommodating the inner tub, and cooling water is disposed between the outer tub and the inner tub to cool the conductive slurry inside the inner tub; Disposed in the inner tub and externally connected to the driving mechanism, the revolving stirrer is used for stirring the conductive slurry in a large path, so that the conductive paste forms a large area displacement inside the inner tub The revolving agitator is an approximately U-shaped or V-shaped frame, and a plurality of blades are arranged on the side of the frame; a self-rotating agitator is used for partially stirring the conductive paste locally; Mainly by the block body rotating along its own axis, so that the conductive paste around the rotating agitator forms a vortex; the self-rotating agitator is a two-turn ball, each of which is suspended by a ball The iron column is suspended and driven by the drive mechanism Each of the trackball is rotated about its own axis of rotation through the center of the sphere, and the conductive paste vortex formation.   如申請專利範圍第1項所述之形成均勻之奈米碳管導電漿料的方法,其中該溼式研磨器包含:一研磨桶,該研磨桶內配置有該導電漿料; 一珠磨攪拌器,係配置在該研磨桶內部,用於將該導電漿料充分的攪拌;多數個研磨珠體,配置在該研磨桶內部,當珠磨攪拌器攪拌時,該研磨珠體會撞擊內部的該導電漿料而將該導電漿料中的奈米碳管充分打散;一過濾器,用於將該研磨桶中的該導電漿料過濾後得到均勻的該導電漿料再往外輸送。  The method for forming a uniform carbon nanotube conductive paste according to claim 1, wherein the wet grinder comprises: a grinding barrel, wherein the polishing barrel is provided with the conductive paste; The inside of the grinding barrel is configured to fully stir the conductive paste; a plurality of grinding beads are disposed inside the grinding barrel, and when the bead mill is stirred, the grinding bead will hit the inside. Conductive slurry to fully disperse the carbon nanotubes in the conductive paste; a filter for filtering the conductive paste in the grinding barrel to obtain a uniform conductive paste and then transporting it outward.   如申請專利範圍第2項所述之形成均勻之奈米碳管導電漿料的方法,其中在該步驟A中,混合及攪拌的時間約15到20分鐘;該第一行星式攪拌器的該公轉式攪拌器的公轉頻率為40rpm(rotation per minute),該第一行星式攪拌器的該自轉式攪拌器為兩顆轉球,其自轉頻率為200rpm,該兩顆轉球為同向旋轉。  The method for forming a uniform carbon nanotube conductive paste according to claim 2, wherein in the step A, the mixing and stirring time is about 15 to 20 minutes; the first planetary agitator The revolution frequency of the revolutionary agitator is 40 rpm (rotation per minute), and the rotary agitator of the first planetary agitator has two rotation balls, and the rotation frequency thereof is 200 rpm, and the two balls rotate in the same direction.   如申請專利範圍第1項所述之形成均勻之奈米碳管導電漿料的方法,其中該分散劑佔該導電漿料的比例在0.8%~1.2%重量百分比之間;該分散劑主要用於將該中型奈米碳管撐開,而不會聚集成一團,甚或下沉到底部,而使得該中型奈米碳管可以在該導電漿料中呈均勻的分布;該分散劑包含高分子分散劑及低分子分散劑;其中該高分子分散劑與低分子分散劑的比例為7:3。  The method for forming a uniform carbon nanotube conductive paste according to claim 1, wherein the proportion of the dispersant to the conductive paste is between 0.8% and 1.2% by weight; the dispersant is mainly used Expanding the medium-sized carbon nanotubes without being aggregated or even sinking to the bottom, so that the medium-sized carbon nanotubes can be uniformly distributed in the conductive paste; the dispersant comprises a polymer a dispersant and a low molecular dispersant; wherein the ratio of the polymer dispersant to the low molecular dispersant is 7:3.   如申請專利範圍第5項所述之形成均勻之奈米碳管導電漿料的方法,其中該高分子分散劑為 PVP(Polyvinylpyrrolidone,聚乙烯吡咯烷酮);其中低分子分散劑為苯磺酸鹽類、溴化銨鹽類及采酮(TritonX-100)。  The method for forming a uniform carbon nanotube conductive paste according to claim 5, wherein the polymer dispersant is PVP (Polyvinylpyrrolidone, polyvinylpyrrolidone); wherein the low molecular dispersant is a besylate , ammonium bromide salts and ketol (Triton X-100).   如申請專利範圍第6項所述之形成均勻之奈米碳管導電漿料的方法,其中該苯磺酸鹽類為任一種苯磺酸鹽類。  The method for forming a uniform carbon nanotube conductive paste according to claim 6, wherein the benzenesulfonate is any one of the besylate salts.   如申請專利範圍第6項所述之形成均勻之奈米碳管導電漿料的方法,其中該溴化銨鹽類為CTAB(cetyltrimethylammonium bromide,溴化十六烷基三甲銨)。  The method for forming a uniform carbon nanotube conductive paste according to claim 6, wherein the ammonium bromide salt is CTAB (cetyltrimethylammonium bromide).   如申請專利範圍第1項所述之形成均勻之奈米碳管導電漿料的方法,其中該中型奈米碳管佔該導電漿料的比例在1%~5%重量百分比之間。  The method for forming a uniform carbon nanotube conductive paste according to claim 1, wherein the medium-sized carbon nanotubes occupies between 1% and 5% by weight of the conductive paste.   如申請專利範圍第2項所述之形成均勻之奈米碳管導電漿料的方法,其中在該步驟B中,混合及攪拌的時間約30到60分鐘,其中該第一行星式攪拌器的該公轉式攪拌器的公轉頻率為40rpm,該第一行星式攪拌器的該自轉式攪拌器為兩顆轉球,其自轉頻率為1200rpm,該兩顆轉球為反向旋轉。  The method for forming a uniform carbon nanotube conductive paste as described in claim 2, wherein in the step B, the mixing and stirring time is about 30 to 60 minutes, wherein the first planetary agitator The revolutionary frequency of the revolutionary agitator is 40 rpm, and the rotary agitator of the first planetary agitator is two rotating balls having a rotation frequency of 1200 rpm, and the two rotating balls are reversely rotated.   如申請專利範圍第2項所述之形成均勻之奈米碳管導電漿料的方法,其中在該步驟C中,混合及攪拌的時間約30到60分鐘,其中該第一行星式攪拌器的該公轉式攪拌器的公轉頻率為40rpm,該第一行星式攪拌器的該自轉式攪拌器為兩顆轉球,其自轉頻率為800rpm,該兩顆轉球為反向旋轉。  The method for forming a uniform carbon nanotube conductive paste according to claim 2, wherein in the step C, the mixing and stirring time is about 30 to 60 minutes, wherein the first planetary agitator The revolutionary frequency of the revolutionary agitator is 40 rpm, and the rotary agitator of the first planetary agitator is two rotating balls, and the rotation frequency thereof is 800 rpm, and the two rotating balls are reversely rotated.   如申請專利範圍第1項所述之形成均勻之奈米碳管導電漿料的方法,其中該石墨烯佔該導電漿料的比例在 0.2%~1.2%重量百分比之間;該石墨烯包含兩種型態,一種為具有二至四層之結構的石墨烯,其佔該導電漿料的比例大於0%重量百分比;另一種則為具有四至八層之結構的石墨烯,其佔該導電漿料的比例大於0%重量百分比,兩種的組合佔該導電漿料的比例在0.2%~1.2%重量百分比之間。  The method for forming a uniform carbon nanotube conductive paste according to claim 1, wherein the ratio of the graphene to the conductive paste is between 0.2% and 1.2% by weight; the graphene comprises two a type of graphene having a structure of two to four layers, the proportion of the conductive paste being more than 0% by weight; and the other being graphene having a structure of four to eight layers, which accounts for the conductive paste The proportion of the material is more than 0% by weight, and the ratio of the two kinds of the conductive paste is between 0.2% and 1.2% by weight.   如申請專利範圍第1項所述之形成均勻之奈米碳管導電漿料的方法,其中該第一製程中的各步驟作用的溫度在20到30℃之間。  A method of forming a uniform carbon nanotube conductive paste as described in claim 1 wherein the temperature in each step of the first process is between 20 and 30 °C.   如申請專利範圍第3項所述之形成均勻之奈米碳管導電漿料的方法,其中在該步驟E中,其中該珠磨攪拌器的轉速為2000到3000rpm,操作溫度小於35℃。  A method of forming a uniform carbon nanotube conductive paste as described in claim 3, wherein in the step E, wherein the bead mill has a rotational speed of 2000 to 3000 rpm and an operating temperature of less than 35 °C.   一種形成均勻之奈米碳管導電漿料的攪拌研磨機構,係將一行星式攪拌器串聯一溼式研磨器,其中該導電漿料先灌注入該行星式攪拌器之後由循環傳送機構讓該導電漿料在該行星式攪拌器及該溼式研磨器之間循環流動;該導電漿料在該行星式攪拌器及該溼式研磨器之間來回流動,應用不同的攪拌及撞擊方式以達到該導電漿料中的奈米碳管的充分分散的效用;其中該導電漿料先在該行星式攪拌器適當的攪拌後,再送入該溼式研磨器,由於該溼式研磨器內的珠磨攪拌器的轉動,該溼式研磨器內的研磨珠體撞擊內部的該導電漿料而將該導電漿料中的奈米碳管充分打散,原來團聚在一起的奈米 碳管,因為該研磨珠體的撞擊而被打散;該導電漿料必須在該行星式攪拌器及該溼式研磨器之間來回流動,應用不同的攪拌及撞擊方式以達到該導電漿料中的奈米碳管的充分分散的效用。  A stirring and grinding mechanism for forming a conductive slurry of uniform carbon nanotubes, wherein a planetary agitator is connected in series with a wet grinder, wherein the conductive paste is first poured into the planetary agitator and then passed by a circulation conveying mechanism The conductive paste circulates between the planetary agitator and the wet grinder; the conductive paste flows back and forth between the planetary agitator and the wet grinder, and different agitation and impact modes are applied to achieve The effect of the sufficient dispersion of the carbon nanotubes in the conductive paste; wherein the conductive paste is first fed to the wet grinder after proper agitation by the planetary agitator, due to the beads in the wet grinder Rotating the agitator, the grinding bead in the wet grinder hits the inner conductive paste to fully dissipate the carbon nanotubes in the conductive paste, and the carbon nanotubes originally reunited together because The abrasive bead is broken by impact; the conductive paste must flow back and forth between the planetary agitator and the wet grinder, and different agitation and impact modes are applied to reach the nanometer in the conductive paste. Carbon tube Fully dispersed utility.   如申請專利範圍第15項所述之形成均勻之奈米碳管導電漿料的攪拌研磨機構,其中該研磨珠體以氧化鋯製作而成。  The agitating and polishing mechanism for forming a uniform carbon nanotube conductive paste according to claim 15 wherein the grinding bead is made of zirconia.   如申請專利範圍第15項所述之形成均勻之奈米碳管導電漿料的攪拌研磨機構,其中該研磨珠體的尺寸介於0.5mm到1.3mm之間。  The agitating grinding mechanism for forming a uniform carbon nanotube conductive paste according to claim 15 wherein the size of the grinding bead is between 0.5 mm and 1.3 mm.   如申請專利範圍第15項所述之形成均勻之奈米碳管導電漿料的攪拌研磨機構,其中該行星式攪拌器包含一公轉式攪拌器,該公轉式攪拌器為一近似U形或V形的框架,並在該框架的側邊配置多數個刀片的結構;攪拌時該公轉式攪拌器沿著該框架的軸線轉動,而使得該導電漿料形成較大路徑的位移。  The agitating grinding mechanism for forming a uniform carbon nanotube conductive paste according to claim 15, wherein the planetary agitator comprises a revolving agitator, and the revolving agitator is an approximate U shape or V The frame is shaped and a plurality of blade structures are disposed on the side of the frame; the agitating agitator rotates along the axis of the frame while stirring, so that the conductive paste forms a displacement of a larger path.   如申請專利範圍第15項所述之形成均勻之奈米碳管導電漿料的攪拌研磨機構,其中該行星式攪拌器包含:一內桶用於放置導電漿料並攪拌該導電漿料;以及一公轉式攪拌器,配置於該內桶內;其中該公轉式攪拌器轉動時所掃出的體積超過該內桶容積之一半。  The agitating grinding mechanism for forming a uniform carbon nanotube conductive paste according to claim 15, wherein the planetary agitator comprises: an inner tub for placing the conductive paste and stirring the conductive paste; A rpm agitator is disposed in the inner tub; wherein the revolutionary agitator rotates a volume that exceeds one half of the inner tub volume.   如申請專利範圍第15項所述之形成均勻之奈米碳管 導電漿料的攪拌研磨機構,其中該行星式攪拌器包含一自轉式攪拌器,該自轉式攪拌器為至少一轉球,各該轉球分別由一懸鐵柱懸吊,再經由驅動機構加以驅動;轉動時該轉球繞著通過其自身球心的軸線轉動,而對該導電漿料形成渦流。  The agitating and grinding mechanism for forming a uniform carbon nanotube conductive paste according to claim 15 , wherein the planetary agitator comprises a self-rotating agitator, wherein the rotary agitator is at least one turning ball, each The ball is suspended by a suspended iron column and driven by a driving mechanism; when rotating, the ball rotates around an axis passing through its own center of the ball to form a eddy current to the conductive paste.   如申請專利範圍第20項所述之形成均勻之奈米碳管導電漿料的攪拌研磨機構,其中該自轉式攪拌器為多個轉球,各個轉球具有相同或不同的旋轉方向。  The agitating grinding mechanism for forming a uniform carbon nanotube conductive paste according to claim 20, wherein the rotating agitator is a plurality of rotating balls, and each of the rotating balls has the same or different rotating directions.  
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CN110775976A (en) * 2019-12-17 2020-02-11 黔西南正胤活性炭科技有限公司 Activation furnace for uniform carbonization and activation
CN113399059A (en) * 2021-06-16 2021-09-17 珠海瑞思普利医药科技有限公司 Wet grinding machine and wet grinding method

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CN104269556B (en) * 2014-09-15 2016-11-09 天奈(镇江)材料科技有限公司 A kind of lithium rechargeable battery CNT and Graphene compound electrocondution slurry

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CN110775976A (en) * 2019-12-17 2020-02-11 黔西南正胤活性炭科技有限公司 Activation furnace for uniform carbonization and activation
CN110775976B (en) * 2019-12-17 2023-09-22 黔西南正胤活性炭科技有限公司 Activation furnace for uniform carbonization and activation
CN113399059A (en) * 2021-06-16 2021-09-17 珠海瑞思普利医药科技有限公司 Wet grinding machine and wet grinding method

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