TW202016348A - An epoxy nano coating and preparation method thereof - Google Patents
An epoxy nano coating and preparation method thereof Download PDFInfo
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本發明涉及等離子體化學氣相沉積技術領域,具體涉及到一種環氧納米塗層及其製備方法。The invention relates to the technical field of plasma chemical vapor deposition, in particular to an epoxy nano-coating and a preparation method thereof.
環氧化合物是指含氧雜環丙烷的化合物,經開環聚合後主鏈中含有醚鍵,具有優良的抗化學品性能,特別是耐酸耐鹼、耐氧化。此外,環氧化合物對眾多基材表面的附著力很好,尤其是金屬表面,經交聯之後,剛性強、耐熱、耐磨;化合物含有三元環醚結構,張力大,熱力學上開環傾向很大,容易形成聚合物,因此環氧樹脂在塗料工業中得到了廣泛應用。CN102229777 A《一種疏水疏油性環氧塗料及其製備和使用方法》通過引入低表面能物質和納米粒子,利用微相分離原理,製備出的環氧塗層具有強疏水疏油性,對水的接觸角可達到149°,對油的接觸角高達101°。其製備方法和使用方法如下:第一步,先將含氟丙烯酸酯、含乙烯基三乙氧基矽烷、苯乙烯等原料按照一定質量配比混合經破乳、水洗和乾燥等多項工藝製備氟矽共聚物;第二步將環氧色漆、製備的氟矽共聚物、混合溶劑、納米二氧化鈣、固化劑等原料按照投料質量配比混合製備得到低表面能環氧塗料;第三步,將該低表面能環氧塗料塗覆在基材表面上上,置於50℃下固化1~5h,再升溫至120℃~200℃下固化1~5h。該方法製備過程複雜,配方中使用多種有機溶劑容易產生污染。CN 107694881 A《一種提高環氧塗層結合強度的方法》提供了一種提高環氧塗層結合強度的方法,即在基體表面進行塗敷環氧樹脂之前,對其進行常壓空氣等離子體處理,將基體表面的油漬、吸附物等轟擊離開表面,增加一些材料基體表面的粗糙度,提高塗層與基體的有效附著面積和浸潤表面積。基體表面經等離子體處理之後2h內,採用刷塗法、噴塗法或流化床法進行環氧塗層的製備。如這兩篇專利所述,目前環氧樹脂的施工工藝都是在基材表面進行液相塗敷,然後採用固化手段使塗層材料進一步交聯形成保護塗層,膜厚一般都在幾十微米以上。但在這個厚度下,塗層本身的阻隔性容易導致基體散熱性、導電性等性能變差。尤其是使用在電子元器件接口等對電子信號要求較高的位置上時,容易出現被處理產品的電子信號大幅衰減,不能正常使用的情況;施工的工藝還決定了這些環氧塗層存在基體表面覆蓋不均勻、器件的部分位置未能被塗層有效保護的情況。利用等離子體成膜方法,可在保持環氧聚合物塗層強度和結合力情況下,實現其厚度在納米和微米級範圍內精確可控。Epoxy compound refers to a compound containing oxirane, which contains ether bond in the main chain after ring-opening polymerization, and has excellent chemical resistance, especially acid resistance, alkali resistance and oxidation resistance. In addition, the epoxy compound has good adhesion to the surface of many substrates, especially the metal surface. After cross-linking, the rigidity is strong, heat-resistant, and wear-resistant; the compound contains a three-membered ring ether structure, high tension, and a tendency to open ring thermodynamically It is very large and easy to form polymers, so epoxy resins are widely used in the coating industry. CN102229777 A "A hydrophobic and oleophobic epoxy coating and its preparation and use method" By introducing low surface energy substances and nanoparticles, using the principle of micro-phase separation, the prepared epoxy coating has strong hydrophobic and oleophobicity and is in contact with water The angle can reach 149°, and the contact angle to oil is up to 101°. The preparation method and use method are as follows: In the first step, fluorine-containing acrylate, vinyl-containing triethoxysilane, styrene and other raw materials are mixed according to a certain mass ratio to prepare fluorine through demulsification, water washing and drying. Silicon copolymer; the second step is to mix the epoxy color paint, prepared fluorosilicone copolymer, mixed solvent, nano calcium dioxide, curing agent and other raw materials according to the mass ratio of the input to prepare a low surface energy epoxy coating; the third step ,Apply the low surface energy epoxy coating on the surface of the substrate, and cure at 50℃ for 1~5h, then heat up to 120℃~200℃ and cure for 1~5h. The preparation process of this method is complicated, and the use of multiple organic solvents in the formulation is prone to pollution. CN 107694881 A "A method for improving the bonding strength of an epoxy coating" provides a method for increasing the bonding strength of an epoxy coating, that is, before applying epoxy resin on the surface of the substrate, it is treated with atmospheric air plasma, Bombing oil stains, adsorbents, etc. from the surface of the substrate away from the surface, increasing the roughness of the surface of some materials, increasing the effective adhesion area and wetting surface area of the coating and the substrate. Within 2 hours after the plasma treatment of the substrate surface, the epoxy coating was prepared by brush coating, spray coating or fluidized bed method. As mentioned in these two patents, the current construction process of epoxy resins is to perform liquid phase coating on the surface of the substrate, and then use curing means to further crosslink the coating material to form a protective coating, the film thickness is generally in the tens of dozens Micron or more. However, at this thickness, the barrier properties of the coating itself can easily lead to poor heat dissipation and conductivity of the substrate. Especially when used in places where electronic signal requirements are high, such as electronic component interfaces, the electronic signal of the processed product is greatly attenuated and cannot be used normally; the construction process also determines the presence of these epoxy coatings. The situation where the surface coverage is uneven and part of the device cannot be effectively protected by the coating. Using the plasma film forming method, the thickness of the epoxy polymer coating can be accurately controlled in the nanometer and micrometer range while maintaining the strength and bonding force of the epoxy polymer coating.
本發明是為了克服以上缺點,提供了利用等離子體化學氣相沉積技術製備環氧樹脂納米塗層的方法及採用該方法獲得的納米塗層。本發明還提供了一種低功率下製備高粘接力塗層的方法。In order to overcome the above shortcomings, the present invention provides a method for preparing epoxy resin nano-coating by using plasma chemical vapor deposition technology and the nano-coating obtained by this method. The invention also provides a method for preparing a high-adhesion coating under low power.
本發明是通過以下技術方案實現的:The present invention is achieved through the following technical solutions:
一種環氧納米塗層,其特徵在於,將基材暴露於具有式(I)所示結構單體,通過等離子體手段在基材表面發生化學反應形成保護塗層:An epoxy nano-coating, characterized in that the substrate is exposed to a monomer having the structure shown in formula (I), and a chemical reaction occurs on the surface of the substrate by plasma means to form a protective coating:
單體:
其中,R1 、R2 、R3 是與三元環相連的基團,獨立地選自氫、烷基、芳基、鹵素、鹵代烷基或羥基;m 為0-8整數,n為1-15的整數。三元環上的基團R1 、R2 、R3 供電特性及基團大小對三元環的穩定性及開環傾向有重要的影響。烷基、芳基、鹵代烷基可作為供電基團穩定三元環,而羥基、鹵素等為吸電子基團則會使三元環中缺電子的碳原子電正性進一步加強,在更低功率等離子體引發下即可迅速開環聚合。Wherein, R 1 , R 2 and R 3 are groups connected to the three-membered ring, and are independently selected from hydrogen, alkyl, aryl, halogen, haloalkyl or hydroxy; m is an integer of 0-8 and n is 1- An integer of 15. The power supply characteristics and group size of the groups R 1 , R 2 and R 3 on the three-membered ring have an important influence on the stability and ring-opening tendency of the three-membered ring. Alkyl, aryl, haloalkyl can be used as a power supply group to stabilize the three-membered ring, while hydroxyl, halogen and other electron-withdrawing groups will further enhance the electron-positive carbon atoms in the three-membered ring. The ring-opening polymerization can be rapidly initiated under the plasma.
進一步地,R1 、R2 、R3 為疏水性基團,獨立地選自氫、烷基、鹵素或鹵代烷基。Further, R 1 , R 2 and R 3 are hydrophobic groups and are independently selected from hydrogen, alkyl, halogen or haloalkyl.
進一步地,所述鹵素為氟,鹵代烷基為碳數在1-10的全氟烷基,所述氟代烷基可以是直鏈,也可以是含有支鏈。Further, the halogen is fluorine, and the haloalkyl group is a perfluoroalkyl group having 1 to 10 carbon atoms. The fluoroalkyl group may be linear or may contain branched chains.
進一步地,所述X為氫或鹵素時,由於碳-氫、碳-鹵素鍵能均較高,單體結構較為穩定、耐化學腐蝕優良。此外,當X優選為氟時,氟原子間作用力大,C-F鍵對稱分佈在整個分子周圍,使分子的表面能很低,聚合得到的塗層具有很好的疏水性。Further, when X is hydrogen or halogen, since the carbon-hydrogen and carbon-halogen bond energies are high, the monomer structure is relatively stable and the chemical resistance is excellent. In addition, when X is preferably fluorine, the interaction force between fluorine atoms is large, the C-F bond is symmetrically distributed around the entire molecule, so that the surface energy of the molecule is very low, and the coating obtained by polymerization has good hydrophobicity.
當m>5、n>10時,單體沸點較高,不利於汽化。優選地,m為0、1、2或3,n為1-8的整數。When m>5, n>10, the boiling point of the monomer is higher, which is not conducive to vaporization. Preferably, m is 0, 1, 2, or 3, and n is an integer of 1-8.
所述的環氧納米塗層可用於對不同基材的表面進行耐化學腐蝕疏水進行防護,基材可以是金屬、光學儀器、衣服織物、電子器件、醫療器械等固體材料。The epoxy nano-coating can be used to protect the surfaces of different substrates against chemical corrosion and hydrophobicity. The substrate can be solid materials such as metals, optical instruments, clothing fabrics, electronic devices, and medical devices.
本發明還公開了一種所述納米塗層的製備方法包括以下步驟:The invention also discloses a preparation method of the nano coating layer including the following steps:
(1)將基材置於等離子體室的反應腔體內,將反應腔體內的真空度抽到0.1-1000毫托;(1) Place the substrate in the reaction chamber of the plasma chamber, and evacuate the vacuum in the reaction chamber to 0.1-1000 mTorr;
(2)通入等離子體源氣體,開啟沉積用等離子體放電將單體經汽化後導入反應腔體進行化學氣相沉積反應;(2) Into the plasma source gas, start the deposition and use plasma discharge to vaporize the monomer into the reaction chamber for chemical vapor deposition reaction;
(3)關閉沉積用等離子體放電,通入潔淨的壓縮空氣或者惰性氣體恢復至常壓,打開腔體,取出基材。(3) Turn off the plasma discharge for deposition, pass clean compressed air or inert gas to return to normal pressure, open the cavity, and remove the substrate.
所述單體是經過減壓汽化後引入反應腔體的。The monomer is introduced into the reaction chamber after being vaporized under reduced pressure.
進一步地,步驟(2)中所述的等離子體源氣體可以是氦氣、氬氣、氮氣、氫氣中的一種或者若干種的混合物。Further, the plasma source gas in step (2) may be one or a mixture of several kinds of helium, argon, nitrogen, and hydrogen.
進一步地,所述等離子體室的容積為1L-2000 L,等離子體源氣體流量為1-1000sccm,通入單體蒸汽的流量為1-2000μL/min。Further, the volume of the plasma chamber is 1L-2000L, the flow rate of the plasma source gas is 1-1000sccm, and the flow rate of the monomer vapor is 1-2000μL/min.
進一步地,所述步驟(2)中,在通入所述等離子體源氣體後以及在所述沉積用等離子體放電之前,還包括對基材進行預處理用等離子體放電工序。Further, in the step (2), after passing the plasma source gas and before the deposition plasma discharge, a plasma discharge step for pretreatment of the substrate is further included.
步驟(2)中通入等離子體源氣體後,開啟預處理等離子體放電先對基材進行預處理。該預處理階段等離子體放電的功率為1-1000W,持續放電時間為1-6000s。After the plasma source gas is introduced in step (2), the pretreatment plasma discharge is turned on and the substrate is pretreated first. The power of plasma discharge in this pretreatment stage is 1-1000W, and the continuous discharge time is 1-6000s.
預處理階段結束後進入沉積階段(預處理用等離子體放電轉換為沉積用等離子體放電),兩個階段的等離子體放電方式以及參數可以相同也可以不同。After the pretreatment phase is completed, the deposition phase is entered (the plasma discharge for pretreatment is converted to a plasma discharge for deposition). The plasma discharge method and parameters of the two phases may be the same or different.
進一步地,所述步驟(2)中,單體導入腔體的過程中沉積用等離子體放電的功率為2-500W,持續放電時間為600-18000s。Further, in the step (2), the power of the plasma discharge for deposition during the introduction of the monomer into the cavity is 2-500 W, and the continuous discharge time is 600-18000 s.
更為優選地,沉積用等離子體放電功率優選2-50W。More preferably, the plasma discharge power for deposition is preferably 2-50W.
進一步地,所述等離子體放電(預處理用等離子體放電和/或沉積用等離子體放電)方式為射頻放電、微波放電、中頻放電、潘寧放電或電火花放電。Further, the plasma discharge (plasma discharge for pretreatment and/or plasma discharge for deposition) is radio frequency discharge, microwave discharge, intermediate frequency discharge, Penning discharge or electric spark discharge.
進一步地,所述等離子體放電(預處理用等離子體放電和/或沉積用等離子體放電)為射頻放電,射頻放電過程中控制等離子體射頻的能量輸出方式為脈衝或連續輸出,等離子體射頻的能量輸出方式為脈衝輸出時,脈寬為10μs-50ms、重複頻率為20Hz-10kHz。Further, the plasma discharge (plasma discharge for pretreatment and/or plasma discharge for deposition) is a radio frequency discharge, and the energy output method for controlling the plasma radio frequency during the radio frequency discharge is pulse or continuous output. When the energy output mode is pulse output, the pulse width is 10μs-50ms and the repetition frequency is 20Hz-10kHz.
與現有技術相比,本發明單體聚合機理為以環氧開環為主,所需激發的等離子體功率低,避免了大功率放電手段對單體分子結構完整性的破壞。本發明採用了與基材的粘接性能很好的環氧化合物,大大提高了納米塗層與基材的結合力。本發明利用等離子體技術引發環氧化合物的聚合反應,通過控制單體流量、等離子體放電功率等工藝條件,避免了環氧化物爆聚導致散熱困難的問題。Compared with the prior art, the monomer polymerization mechanism of the present invention is based on epoxy ring opening, and the plasma power required for excitation is low, which avoids the destruction of the monomer molecular structure integrity by high-power discharge means. The invention adopts an epoxy compound with good adhesion to the substrate, which greatly improves the binding force between the nano coating and the substrate. The invention uses the plasma technology to initiate the polymerization reaction of the epoxy compound. By controlling the process conditions such as monomer flow rate and plasma discharge power, the problem of difficulty in heat dissipation caused by the explosive polymerization of the epoxide is avoided.
實施例Examples 11
一種環氧納米塗層及其製備方法,經過如下步驟:An epoxy nano-coating and its preparation method go through the following steps:
(1)將鐵塊放置於200L等離子體真空反應腔體內,對反應腔體連續抽真空使真空度達到0.8毫托。(1) Place the iron block in the 200L plasma vacuum reaction chamber, and continuously evacuate the reaction chamber to achieve a vacuum of 0.8 mtorr.
(2)通入氦氣,流量為50sccm,開啟射頻等離子體放電對鐵塊基材進行預處理(即開啟射頻方式的預處理用等離子體放電),預處理階段放電功率為20W,持續放電100 s。(2) Introduce helium gas with a flow rate of 50sccm. Turn on the RF plasma discharge to pretreat the iron base material (that is, turn on the RF pretreatment plasma discharge). The discharge power in the pretreatment stage is 20W, and the continuous discharge is 100. s.
(3)通入單體S1在基材表面進行化學氣相沉積製備納米塗層,單體流量為150 μL/min,經過1毫托高真空汽化後通入反應腔體,通入時間為2000s。預處理用等離子體放電調整為沉積用等離子體放電。該沉積階段腔體內等離子體的產生採用射頻放電方式,輸出方式為脈衝,脈衝寬度為5μs,重複頻率為3000Hz,放電功率為10W,放電時間為2000s。(3) The monomer S1 is passed through the chemical vapor deposition on the surface of the substrate to prepare a nano-coating, the monomer flow rate is 150 μL/min, after 1 mtorr high vacuum vaporization, it is passed into the reaction chamber, and the passing time is 2000s . The plasma discharge for pretreatment is adjusted to the plasma discharge for deposition. The plasma in the deposition stage is generated by radio frequency discharge, the output mode is pulse, the pulse width is 5 μs, the repetition frequency is 3000 Hz, the discharge power is 10 W, and the discharge time is 2000 s.
(4)塗層製備結束後,通入氮氣,使反應腔體恢復至常壓,打開腔體,取出金屬鐵塊。(4) After the coating preparation is completed, nitrogen gas is introduced to restore the reaction chamber to normal pressure, the chamber is opened, and the metal iron block is removed.
(5)對樣品塗層防護性能進行檢測,檢測內容包括塗層厚度、疏水性(水接觸角)、耐化學腐蝕情況、塗層附著力、接觸電阻。
單體S1Monomer S1
其中,預處理用等離子體放電裝置和沉積用等離子體放電裝置可以是一套,也可以為獨立的兩套裝置。預處理用等離子體放電裝置(例如電極)優選地設置在反應腔體內,且圍繞基材設置,從而便於預處理後快速與塗層工藝銜接;沉積用等離子體放電裝置可以佈設在反應腔體之外且遠離反應腔體設置,從而可選擇地或盡可能地避免塗層過程中等離子體放電對基材的消極影響。Among them, the plasma discharge device for pretreatment and the plasma discharge device for deposition may be one set or two separate sets. The plasma discharge device (for example, electrode) for pretreatment is preferably arranged in the reaction chamber and around the base material, so as to facilitate the quick connection with the coating process after pretreatment; the plasma discharge device for deposition can be arranged in the reaction chamber It is installed outside and away from the reaction chamber, so as to avoid the negative influence of the plasma discharge on the substrate during the coating process selectively or as far as possible.
實施例Examples 22
一種環氧納米塗層及其製備方法,經過如下步驟:An epoxy nano-coating and its preparation method go through the following steps:
(1)將鎂合金放置於800L等離子體真空反應腔體內,對反應腔體連續抽真空使真空度達到50毫托。(1) Place the magnesium alloy in the 800L plasma vacuum reaction chamber, and continuously evacuate the reaction chamber to achieve a vacuum of 50 mTorr.
(2)通入氦氣,流量為50sccm,開啟射頻等離子體放電對鎂合金基材進行預處理(即開啟射頻方式的預處理用等離子體放電),預處理階段放電功率為20W,持續放電100 s。(2) Introduce helium gas with a flow rate of 50sccm. Turn on the radio frequency plasma discharge to pretreat the magnesium alloy substrate (that is, turn on the radio frequency mode pretreatment plasma discharge). The discharge power in the pretreatment stage is 20W, and the continuous discharge is 100 s.
(3)通入單體S2在基材表面進行化學氣相沉積製備納米塗層,單體流量為300 μL/min,經過10毫托高真空汽化後通入反應腔體,通入時間為2500s。預處理用等離子體放電調整為沉積用等離子體放電。(3) The monomer S2 is passed through the chemical vapor deposition on the surface of the substrate to prepare a nano-coating, the monomer flow rate is 300 μL/min, after 10 mTorr high vacuum vaporization, it is passed into the reaction chamber, and the passing time is 2500s . The plasma discharge for pretreatment is adjusted to the plasma discharge for deposition.
該沉積階段腔體內等離子體的產生採用射頻放電方式,輸出方式為脈衝,脈衝寬度為100μs,重複頻率為5000Hz,放電功率為20W,放電時間為2500s。(4)塗層製備結束後,通入氮氣,使反應腔體恢復至常壓,打開腔體,取出鎂合金。(5)對樣品塗層防護性能進行檢測,檢測內容包括塗層厚度、疏水性(水接觸角)、耐化學腐蝕、塗層附著力、接觸電阻。
單體S2Monomer S2
實施例Examples 33
與實施例1相比,步驟(1)抽真空至100 毫托;步驟(2)中單體S1更換為單體S3,步驟(3)單體通入時間、放電時間更換為3000s,其他條件相同。
單體S3Single S3
實施例Examples 44
與實施例1相比,步驟(1)抽真空至150 毫托;步驟(2)中單體S1更換為單體S4,步驟(3)單體通入時間和放電時間更換為3500s,其他條件相同。
單體S4Single S4
實施例Examples 55
與實施例2相比,步驟(2)氦氣改為氮氣;步驟(2)中單體S1更換為單體S5,步驟(3)單體通入時間、放電時間更換為4000s,其他條件相同。
單體S5Single S5
實施例Examples 66
與實施例1相比,將單體S1更換為S2,其他條件相同。Compared with Example 1, the monomer S1 was replaced with S2, and other conditions were the same.
實施例Examples 77
與實施例2相比,將基材更換為手機PCB板,其他條件相同。Compared with Example 2, the substrate is replaced with a mobile phone PCB board, and other conditions are the same.
實施例Examples 88
與實施例2相比,將步驟(3)中的放電功率更換為5W,其他條件相同Compared with Example 2, the discharge power in step (3) was changed to 5W, and other conditions were the same
實施例Examples 99
與實施例2相比,將步驟(3)中的單體通入時間、放電時間均更換為12000s,其他條件相同。Compared with Example 2, the monomer inflow time and discharge time in step (3) are both changed to 12000s, and other conditions are the same.
實施例Examples 1010
與實施例2相比,將步驟(3)中的單體流量更換為800 μL/min,其他條件相同。Compared with Example 2, the monomer flow rate in step (3) was changed to 800 μL/min, and other conditions were the same.
將上述各實施例施鍍後的基材,進行塗層厚度、水接觸角、耐鹼性銹蝕、附著力接觸阻值的測試。The substrates after the plating in the above embodiments were tested for coating thickness, water contact angle, alkali corrosion resistance, and adhesion contact resistance.
納米塗層厚度,使用美國Filmetrics-F20-UV-薄膜厚度測量儀進行檢測。The thickness of the nano-coating is tested using the US Filmetrics-F20-UV-film thickness measuring instrument.
納米塗層水接觸角,根據GB/T 30447-2013標準進行測試。Nano-coating water contact angle, tested according to GB/T 30447-2013 standard.
耐化學腐蝕,參照GB1763-79(89)漆膜耐化學試劑性測定法標準進行測試。附著力測試方法,根據GB/T 9286-1998標準進行百格刀劃格試驗。For chemical resistance, refer to GB1763-79(89) Paint Film Chemical Resistance Determination Standard for testing. Adhesion test method, according to GB/T 9286-1998 standard for 100 grid knife scratch test.
接觸阻值的測試方法,參照GB/T5095.2-1997進行測試。For the test method of contact resistance, refer to GB/T5095.2-1997 for testing.
表1
採用本技術方案製備環氧塗層過程,與傳統液相法相比,不需要使用固化劑、有機溶劑等環境污染物,且本技術製備得到的塗層可在納米尺度範圍實現耐鹼、高粘附,同時接觸電阻非常低。在電子產品連接處,所塗覆的塗層具有優良的導通性是一個關鍵性指標;傳統方法製備的塗層厚達幾十微米,電阻很大,不能應用於電子產品的連接部位。Compared with the traditional liquid phase method, the process of preparing the epoxy coating by this technical solution does not require the use of environmental pollutants such as curing agents and organic solvents, and the coating prepared by this technology can achieve alkali resistance and high viscosity in the nanometer range Attached, while the contact resistance is very low. At the connection of electronic products, the excellent conductivity of the applied coating is a key indicator; the coating prepared by the traditional method is tens of microns thick and has a large resistance, which cannot be applied to the connection of electronic products.
最後應說明的是:以上各實施例僅用以說明本發明的技術方案,而非對其限制;儘管參照前述各實施例對本發明進行了詳細的說明,本領域的普通技術人員應當理解:其依然可以對前述各實施例所記載的技術方案進行修改,或者對其中部分或者全部技術特徵進行等同替換;而這些修改或者替換,並不使相應技術方案的本質脫離本發明各實施例技術方案的範圍。Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention, rather than limiting it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: The technical solutions described in the foregoing embodiments can still be modified, or some or all of the technical features can be equivalently replaced; and these modifications or replacements do not deviate from the essence of the corresponding technical solutions of the technical solutions of the embodiments of the present invention. range.
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