TW201827358A - Method for preparing porous material - Google Patents

Method for preparing porous material Download PDF

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TW201827358A
TW201827358A TW106103266A TW106103266A TW201827358A TW 201827358 A TW201827358 A TW 201827358A TW 106103266 A TW106103266 A TW 106103266A TW 106103266 A TW106103266 A TW 106103266A TW 201827358 A TW201827358 A TW 201827358A
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mixture
weight
porous material
sludge
chemical mechanical
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TW106103266A
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TWI619680B (en
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廖三棨
江世哲
鄭瑞濱
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潤泰精密材料股份有限公司
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Priority to CN201710242626.7A priority patent/CN108358607A/en
Priority to JP2017088284A priority patent/JP6379252B2/en
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Abstract

The present invention provides a method for preparing a porous material, comprising: providing a dry sludge generated by chemical mechanical polishing in a semiconductor process; mixing and grinding the dry sludge, a clay mineral and a foaming agent to form a powder; mixing the powder and a binding agent to obtain a mixture; and then bloating the mixture at high temperature to obtain the porous material.

Description

製備多孔性材料的方法  Method for preparing porous material  

本發明係關於一種製備多孔性材料的方法,其特徵在於,將半導體製程中化學機械研磨所產生之污泥轉化成多孔性材料。 The present invention relates to a method of producing a porous material, which is characterized in that a sludge produced by chemical mechanical polishing in a semiconductor process is converted into a porous material.

輕質骨材最早源自西元1908年,美國利用膨脹性黏土及頁岩,經過旋窯於高溫下燒製獲得。而燒製輕質骨材的原料選擇上,有天然的原料如珍珠岩、松脂岩、頁岩、板岩及蛭石等,但因天然原料的獲得需進行礦物開採,對於環境的破壞較大且此類礦物匱乏之國家亦不容易發展輕質骨材。於1970年代開始,輕質骨材的原料發展有選用工業廢棄物,如膨脹礦渣、煤矸石陶粒、粉煤灰、下水道汙泥、工業汙泥以及飛灰等;在台灣直至1990年代,始之利用水庫淤泥作為製造輕質骨材以發展輕質混凝土。 Lightweight aggregates originated in 1908. The United States used expansive clay and shale to be fired at high temperatures in a rotary kiln. In the selection of raw materials for burning lightweight aggregates, there are natural raw materials such as perlite, rosin rock, shale, slate and vermiculite. However, due to the acquisition of natural raw materials, mineral mining is required, and the damage to the environment is large. It is also not easy for countries with such mineral scarcity to develop lightweight aggregates. Since the 1970s, the development of raw materials for lightweight aggregates has selected industrial wastes such as expanded slag, coal gangue ceramsite, fly ash, sewage sludge, industrial sludge and fly ash; in Taiwan until the 1990s, The use of reservoir sludge as a lightweight aggregate to develop lightweight concrete.

因此隨著製備輕質骨材所使用的原料不同,故製程上也會有所差別。最初的輕質骨材之製作法係選擇自然界礦物作為原料,如頁岩或膨脹黏土,礦物經過開採後,破碎篩分至適當粒徑的大小後進入旋窯燒結膨脹,完成品需再經過破碎分級出產品別。依據生產商的不同,過程中會進行造粒動作(pelletizing),使骨材形成大小約5mm至20mm圓形造粒體, 依照造粒體的大小差異具有不同的產品別,圓形造粒體主要係因可幫助混凝土在高壓輸送的流動性,故具低吸水性之圓形骨材較受業界所採用。如原料取用工業廢棄物,為維持成分的均一性,製程中需加入配料措施(ingredient)以維持後續燒製膨脹的溫度條件,其中德國Dennert Poraver公司係利用廢棄玻璃進行膨脹骨材的生產,除生產5mm至10mm之輕質骨材,並於西元2003年成功利用噴霧造粒生產超細輕質骨材,最小粒徑可至0.04mm,因粒徑範圍的延伸,骨材除應用在生產輕質混凝土,亦可添加至塗料中,可見輕質骨材不止於建築材料的應用。 Therefore, as the materials used to prepare the lightweight aggregates are different, the process will vary. The original method of making lightweight aggregates uses natural minerals as raw materials, such as shale or expanded clay. After mining, the minerals are crushed and sieved to the appropriate size and then enter the rotary kiln for sintering and expansion. Out of the product. Depending on the manufacturer, the pelletizing process is carried out during the process, so that the aggregate forms a circular granule of about 5 mm to 20 mm in size, which has different products depending on the size of the granule, circular granules. The main reason is that it can help the concrete to flow at high pressure, so the circular aggregate with low water absorption is more used by the industry. If the raw materials are used for industrial waste, in order to maintain the uniformity of the ingredients, the ingredients need to be added in the process to maintain the temperature conditions for subsequent firing and expansion. The German Dennert Poraver Company uses waste glass for the production of expanded aggregates. In addition to the production of lightweight aggregates from 5mm to 10mm, and successfully used spray granulation in 2003 to produce ultra-fine lightweight aggregates, the minimum particle size can reach 0.04mm. Due to the extension of the particle size range, the aggregates are used in production. Lightweight concrete can also be added to the coating, showing that lightweight aggregates are not limited to building materials.

此外,製備輕質骨材時,需經過一燒製程序,使其發生膨脹行為而形成多孔結構。先前研究指出只要符合一定成份範圍的二氧化矽(SiO2)、氧化鋁(Al2O3)及助熔劑(氧化鈉(Na2O)、氧化鉀(K2O)、氧化鈣(CaO)、氧化鎂(MgO)、氧化鐵(Fe2O3)),燒製溫度約在1100℃至1300℃可達到發泡的效應,其中SiO2影響玻璃相的黏度,含量越高時,所得到的玻璃相之黏度也隨之提升,對骨材的性質影響,則是降低骨材的強度;氧化鋁則是影響骨材強度與密度;其他助熔劑影響玻璃相之黏度,含量增加時,玻璃相的黏度隨之下降。根據其他研究顯示,輕質骨材的製造過程一定要滿足兩種條件:(1)原料加熱至高溫時,必須能夠生成黏性的玻璃相來包覆逸散的氣體;當玻璃相黏滯度較高時,所產生的孔隙較細,黏滯度低時,產生在內部的孔洞較大;以及(2)在原料內部氣體生成前,表面必須以生成玻璃相。 In addition, when preparing lightweight aggregates, a firing process is required to cause expansion to form a porous structure. Previous studies have indicated that cerium oxide (SiO 2 ), aluminum oxide (Al 2 O 3 ) and flux (sodium oxide (Na 2 O), potassium oxide (K 2 O), calcium oxide (CaO)) can be used as long as they meet a certain range of composition. , magnesium oxide (MgO), iron oxide (Fe 2 O 3 )), firing temperature of about 1100 ° C to 1300 ° C can achieve the effect of foaming, wherein SiO 2 affects the viscosity of the glass phase, the higher the content, the The viscosity of the glass phase is also increased. The influence on the properties of the aggregate is to reduce the strength of the aggregate; the alumina affects the strength and density of the aggregate; the other flux affects the viscosity of the glass phase, and when the content increases, the glass The viscosity of the phase decreases. According to other studies, the manufacturing process of lightweight aggregates must meet two conditions: (1) When the raw material is heated to high temperature, it must be able to form a viscous glass phase to cover the fugitive gas; when the glass phase viscosity At higher levels, the resulting pores are finer, and when the viscosity is low, the pores generated inside are large; and (2) the surface must be formed to form a glass phase before the gas inside the raw material is generated.

而因輕質骨材為一種具多孔結構的礦物粒料,可經由高溫燒 製獲得,故具耐火性質,且因其結構關係,具有隔音、隔熱且質輕的效果,依照物理特性用於結構混凝土及非結構性混凝土的用途上,如道路瀝青料、高樓建築之結構樑或是隔音牆面。 Because the lightweight aggregate is a porous mineral material, it can be obtained by high-temperature firing, so it has fire-resistance properties, and because of its structural relationship, it has sound insulation, heat insulation and light weight effect, and is used according to physical properties. The use of structural concrete and non-structural concrete, such as road asphalt, structural beams of high-rise buildings or soundproof walls.

目前隨著半導體工業的發展,晶圓尺寸的需求已經從8吋上升到12吋,為了在晶圓上累積更多的元件,晶圓的平坦化措施已是一項標準化流程,化學機械研磨(Chemical-Mechanical Polishing;CMP)製法是目前主要使晶圓平整的方式,而在CMP研磨液中,參雜了許多奈米級二氧化矽(SiO2)粒子作為研磨粒體,於製程使用完畢後,懸浮在廢水之中,為了減少環境衝擊及符合廢水排放標準,CMP製程廢水經過一定處理程序及過濾後,產生許多由奈米粒子及絮凝物所組成的汙泥,其狀況多為餅狀並依據絮凝物的種類而有白色及棕色之分。 With the development of the semiconductor industry, the demand for wafer size has increased from 8吋 to 12吋. In order to accumulate more components on the wafer, wafer flattening has become a standardized process, chemical mechanical polishing ( The Chemical-Mechanical Polishing; CMP) method is currently the main method of flattening the wafer. In the CMP slurry, many nano-sized cerium oxide (SiO 2 ) particles are mixed as abrasive granules. Suspended in waste water, in order to reduce environmental impact and meet wastewater discharge standards, CMP process wastewater has a number of sludges composed of nano particles and floes after a certain treatment process and filtration. The type of floc is white and brown.

目前CMP汙泥的處理方式,多為掩埋,其極微細尺寸的顆粒倘若懸浮至水體中,更易因濁度問題導致二次汙染,選擇掩埋的原因係因為未有完善的再利用方式來處理CMP汙泥,使其資源化再利用。 At present, the treatment of CMP sludge is mostly buried. If the particles of extremely fine size are suspended in the water body, it is more likely to cause secondary pollution due to turbidity problems. The reason for choosing to bury is because there is no perfect recycling method to treat CMP. The sludge is recycled and reused.

是以,CMP汙泥含有高量之二氧化矽(SiO2)的成份,因此若能透過特別的製程,將其轉化成再生材料,將有助於環境保護以及資源的再利用。 Therefore, CMP sludge contains a high amount of cerium oxide (SiO 2 ), so if it can be converted into a recycled material through a special process, it will contribute to environmental protection and resource reuse.

本發明之主要目的即在提供一種利用事業廢棄物為材料之再生骨材及其再生方法,其以半導體廠製造晶圓時以化學機械研磨 (Chemical-Mechanical Polishing;CMP)製程所產生出來的事業廢棄物(如汙泥),藉由添加其他物質改變其化學組成,再經過燒結膨脹後,可轉化成輕質骨材。該輕質骨材具有隔熱、質輕及吸水等特性,可用於營建混凝土工程之用。故本發明之產物具有減廢、資源再利用之環境保護效益。 A main object of the present invention is to provide a regenerated aggregate using a business waste as a material and a method for regenerating the same, which is produced by a chemical-mechanical polishing (CMP) process when a wafer is manufactured by a semiconductor factory. Waste (such as sludge) can be converted into light aggregate by adding other substances to change its chemical composition and then sintering and expanding. The lightweight aggregate has the characteristics of heat insulation, light weight and water absorption, and can be used for concrete construction. Therefore, the product of the invention has the environmental protection benefits of waste reduction and resource reuse.

本文中的用語「一」或「一種」係用以敘述本發明之元件及成分。此術語僅為了敘述方便及給予本發明之基本觀念。此敘述應被理解為包括一種或至少一種,且除非明顯地另有所指,表示單數時亦包括複數。於申請專利範圍中和”包含”一詞一起使用時,該用語「一」可意謂一個或超過一個。 The articles "a" or "an" are used herein to describe the elements and compositions of the invention. This terminology is only for convenience of description and the basic idea of the invention. This description is to be construed as inclusive of the singular When used in conjunction with the word "comprising", the term "a" may mean one or more than one.

本文中的用語「或」其意同「及/或」。 The term "or" in this document means "and/or".

緣是,為達成前述之目的,本發明提供一種製備多孔性材料的方法,其包含:(1)提供一乾燥的半導體製程中化學機械研磨所產生之污泥;(2)將該乾燥的半導體製程中化學機械研磨所產生之污泥及一黏土礦物混合,得一第一混合物,再添加一發泡劑於該第一混合物中,並研磨成粉體,得一第二混合物;(3)將該第二混合物與一黏結劑混合,得一第三混合物;以及(4)燒結膨脹該第三混合物,得一多孔性材料。 In order to achieve the foregoing objects, the present invention provides a method of preparing a porous material comprising: (1) providing a sludge produced by chemical mechanical polishing in a dry semiconductor process; and (2) drying the semiconductor The sludge produced by the chemical mechanical polishing in the process is mixed with a clay mineral to obtain a first mixture, a foaming agent is added to the first mixture, and ground into a powder to obtain a second mixture; (3) The second mixture is mixed with a binder to obtain a third mixture; and (4) sintered to expand the third mixture to obtain a porous material.

半導體產業晶圓製造加工過程中之化學機械研磨與濕式酸洗,會產生化學機械研磨液污泥(chemical mechanical polishing sludge;CMP污泥),其為事業廢棄物,因該CMP污泥含有多種之氧化劑、添加劑、分散劑、研磨緩衝之有機與無機化合物等,其中更含有大量奈米級之二氧化矽(SiO2)、氧化鋁(Al2O3)等微粒子。同時該CMP污泥會含有大量水分 (含水率約55至70%),因此需將該CMP污泥乾燥(例如熱風烘乾),使之含水率低於5%以下,再進行後續製程。故本發明的「乾燥的半導體製程中化學機械研磨所產生之污泥」係指乾燥來自半導體晶圓製造廠產生之CMP污泥而得。於一具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥之含水率低於5%以下。於一較佳具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥之含水率低於3%以下。於一更佳具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥之含水率低於1%以下。於一具體實施例中,本發明之方法進一步包含一步驟(1’),其施行於步驟(1)之前,其包含提供一半導體製程中化學機械研磨所產生之污泥,並乾燥該半導體製程中化學機械研磨所產生之污泥,以得一乾燥的半導體製程中化學機械研磨所產生之污泥。 Chemical mechanical polishing and wet pickling in the wafer manufacturing process of the semiconductor industry generate chemical mechanical polishing sludge (CMP sludge), which is a commercial waste, because the CMP sludge contains various The oxidizing agent, the additive, the dispersing agent, the organic and inorganic compound of the grinding buffer, and the like, and further contain a large amount of fine particles such as nanometer-sized cerium oxide (SiO 2 ) or aluminum oxide (Al 2 O 3 ). At the same time, the CMP sludge will contain a large amount of water (water content of about 55 to 70%), so the CMP sludge needs to be dried (for example, hot air drying) so that the water content is less than 5%, and then the subsequent process is carried out. Therefore, the "sludge produced by chemical mechanical polishing in a dry semiconductor process" of the present invention is obtained by drying CMP sludge produced from a semiconductor wafer manufacturing plant. In one embodiment, the moisture produced by the chemical mechanical polishing in the dry semiconductor process has a moisture content of less than 5%. In a preferred embodiment, the moisture produced by the chemical mechanical polishing in the dry semiconductor process has a moisture content of less than 3%. In a more preferred embodiment, the moisture produced by the chemical mechanical polishing in the dry semiconductor process has a moisture content of less than 1%. In a specific embodiment, the method of the present invention further comprises a step (1'), which is performed prior to the step (1), comprising providing a sludge produced by chemical mechanical polishing in a semiconductor process, and drying the semiconductor process The sludge produced by the chemical mechanical grinding process is used to obtain the sludge produced by chemical mechanical polishing in a dry semiconductor process.

於另一具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥中二氧化矽含量為60%以上。於一較佳具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥中二氧化矽含量為65%以上。於一更佳具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥中二氧化矽含量為70%以上。 In another embodiment, the amount of cerium oxide in the sludge produced by chemical mechanical polishing in the dry semiconductor process is 60% or more. In a preferred embodiment, the amount of cerium oxide in the sludge produced by chemical mechanical polishing in the dry semiconductor process is 65% or more. In a more preferred embodiment, the amount of cerium oxide in the sludge produced by chemical mechanical polishing in the dry semiconductor process is 70% or more.

本文中「黏土礦物」一詞包含但不限於層狀矽酸鹽礦物。於一具體實施例中,該黏土礦物包含一高嶺土、一膨潤土、一雲母、一葉蠟石、一綠土、一蛭石以及一滑石。於一較佳具體實施例中,該黏土礦物為一高嶺土。 The term "clay mineral" as used herein includes, but is not limited to, layered citrate minerals. In one embodiment, the clay mineral comprises a kaolin, a bentonite, a mica, a pyrophyllite, a smectite, a vermiculite, and a talc. In a preferred embodiment, the clay mineral is a kaolin.

本文中「發泡劑」一詞包含但不限於一碳酸化合物。於一具體 實施例中,該發泡劑包含一碳酸鈉、一碳酸氫鈉、一過碳酸鈉、一過碳酸鈣以及一碳酸鈣。於一較佳具體實施例中,該發泡劑為一碳酸鈉或一碳酸鈣。 The term "foaming agent" as used herein includes, but is not limited to, a monocarbonate. In one embodiment, the blowing agent comprises sodium carbonate, sodium hydrogencarbonate, sodium percarbonate, monocalcium carbonate, and calcium carbonate. In a preferred embodiment, the blowing agent is sodium carbonate or calcium carbonate.

於一具體實施例中,該乾燥的半導體製程中化學機械研磨所產生之污泥占該第一混合物的重量百分比為85%至95%。於另一具體實施例中,該黏土礦物占該第一混合物的重量百分比為5%至15%。於一具體實施例中,該發泡劑的添加量為該第一混合物之總重量的0.5%至8%。 In one embodiment, the sludge produced by the chemical mechanical polishing in the dry semiconductor process comprises from 85% to 95% by weight of the first mixture. In another embodiment, the clay mineral comprises from 5% to 15% by weight of the first mixture. In one embodiment, the blowing agent is added in an amount from 0.5% to 8% by total weight of the first mixture.

本發明將該第一混合物和該發泡劑一起混合後,將其研磨以獲得粉體狀之該第二混合物,而該「研磨」可採用習知的研磨方式,而不需加以限制,較佳為球磨。而將研磨後所得之粉體狀之第二混合物要進行過篩,過篩的目的係為獲得粒徑平均較小的粉體顆粒,其將有助於後續和黏結劑反應時能均勻攪拌混合。本發明使用100至200號篩網過篩;較佳地,係使用200號篩網。較佳地,經前述過篩步驟後,所篩選的粉體顆粒之粒徑小於150μm;更佳地,所篩選的粉體顆粒之粒徑小於75μm。於一具體實施例中,本發明之方法進一步包含一步驟(2’),其位於步驟(2)以及(3)之間,其包含過篩該第二混合物,以使該第二混合物之粉體顆粒之粒徑小於150μm。 After the first mixture and the foaming agent are mixed together, the first mixture is ground to obtain the powdery second mixture, and the "grinding" can be carried out by a conventional grinding method without limitation. Good for ball milling. The second mixture of the powder obtained after the grinding is sieved, and the purpose of the sieving is to obtain powder particles having a smaller average particle diameter, which will facilitate uniform mixing and mixing after the reaction with the binder. . The present invention uses a 100 to 200 mesh screen; preferably, a 200 mesh screen is used. Preferably, after the sieving step, the particle size of the powder particles to be screened is less than 150 μm; more preferably, the particle size of the powder particles to be screened is less than 75 μm. In a specific embodiment, the method of the present invention further comprises a step (2') between steps (2) and (3) comprising sieving the second mixture to make the powder of the second mixture The particle size of the bulk particles is less than 150 μm.

本文中「黏結劑」一詞包含但不限於具有使粉體(如粉體狀之第二混合物)相互黏接成一塊的功能之溶劑。於一具體實施例中,該黏結劑占該第三混合物的重量百分比為18%至60%。 The term "adhesive" as used herein includes, but is not limited to, a solvent having the function of bonding powders (e.g., a second mixture of powders) to each other. In one embodiment, the binder comprises from 18% to 60% by weight of the third mixture.

於另一具體實施例中,該黏結劑包含一鹼金屬化合物溶液或 一鹼土金屬化合物溶液。本文中「鹼金屬化合物溶液」一詞係指一含有鹼金屬離子(如鋰離子、鈉離子或鉀離子等)之溶液。於一具體實施例中,該鹼金屬化合物溶液為一鹼金屬氫氧化物溶液或一鹼金屬氧化物溶液。於一較佳具體實施例中,該鹼金屬氫氧化物溶液為一氫氧化鈉溶液。本文中「鹼土金屬化合物溶液」一詞係指一含有鹼土金屬離子(如鈹離子、鎂離子或鈣離子等)之溶液。於一具體實施例中,該鹼土金屬化合物溶液為一鹼土金屬氫氧化物溶液或一鹼土金屬氧化物溶液。於一較佳具體實施例中,該鹼土金屬氫氧化物溶液為一氫氧化鈣溶液。 In another embodiment, the binder comprises an alkali metal compound solution or an alkaline earth metal compound solution. The term "alkali metal compound solution" as used herein refers to a solution containing an alkali metal ion such as lithium ion, sodium ion or potassium ion. In one embodiment, the alkali metal compound solution is an alkali metal hydroxide solution or an alkali metal oxide solution. In a preferred embodiment, the alkali metal hydroxide solution is a sodium hydroxide solution. The term "alkaline earth metal compound solution" as used herein refers to a solution containing an alkaline earth metal ion such as barium ion, magnesium ion or calcium ion. In one embodiment, the alkaline earth metal compound solution is an alkaline earth metal hydroxide solution or an alkaline earth metal oxide solution. In a preferred embodiment, the alkaline earth metal hydroxide solution is a calcium hydroxide solution.

本發明將該第二混合物與一黏結劑混合後會形成一膏狀物(即第三混合物)。此時使用者可依據往後產品需求,將該膏狀物進行造粒,即切成所需要的尺寸大小,例如1或3mm粒徑之顆粒,再進行燒結膨脹的動作;或是直接將該膏狀物不造粒進行燒結膨脹。於一具體實施例中,本發明之方法進一步包含一步驟(3”),其接於步驟(3)及(4)中間,其包含對該第三混合物進行造粒,即將該第三混合物切成一定尺寸大小之顆粒。於一具體實施例中,該造粒係將該第三混合物切成粒徑小於5mm之顆粒。於一較佳具體實施例中,該造粒係將該第三混合物切成粒徑小於3mm之顆粒。於一更佳具體實施例中,該造粒係將該第三混合物切成粒徑小於1mm之顆粒。 The second mixture of the present invention is mixed with a binder to form a paste (i.e., a third mixture). At this time, the user can granulate the paste according to the requirements of the product in the future, that is, cut into a desired size, for example, a particle having a particle size of 1 or 3 mm, and then perform a sintering expansion operation; or directly The paste is not granulated for sintering expansion. In a specific embodiment, the method of the present invention further comprises a step (3"), which is carried out in the middle of steps (3) and (4), comprising granulating the third mixture, ie cutting the third mixture Particles of a certain size. In one embodiment, the granulation cuts the third mixture into particles having a particle size of less than 5 mm. In a preferred embodiment, the granulation system is the third mixture. The granules are cut into particles having a particle size of less than 3 mm. In a more preferred embodiment, the granulation system cuts the third mixture into granules having a particle size of less than 1 mm.

本文中的「燒結膨脹」一詞包含利用高溫爐進行燒結膨脹,其中該高溫爐包含一電窯、一瓦斯窯以及一材窯。本發明不對該第三混合物或造粒後之第三混合物進行乾燥動作而直接進行燒結膨脹,其燒結膨脹的 溫度範圍為400℃至800℃;較佳地,該燒結膨脹的溫度範圍為500℃至700℃;更佳地,該燒結膨脹的溫度範圍為500℃至600℃。該第三混合物或造粒後之第三混合物不進行乾燥而直接進行燒結膨脹,所得為一高吸水性的多孔性材料。因此,於一具體實施例中,該多孔性材料之吸水率為70wt%以上;較佳地,該吸水率為80wt%以上;更佳地,該吸水率為90wt%以上。 The term "sintering expansion" as used herein encompasses the use of a high temperature furnace for sintering expansion, wherein the high temperature furnace comprises an electric kiln, a gas kiln and a kiln. The present invention does not directly perform the sintering expansion of the third mixture or the third mixture after granulation, and the sintering expansion temperature ranges from 400 ° C to 800 ° C; preferably, the sintering expansion temperature ranges from 500 ° C To 700 ° C; more preferably, the sintering expands at a temperature in the range of 500 ° C to 600 ° C. The third mixture or the third mixture after granulation is directly sintered and expanded without drying, and is obtained as a highly water-absorptive porous material. Therefore, in one embodiment, the water absorption of the porous material is 70% by weight or more; preferably, the water absorption is 80% by weight or more; more preferably, the water absorption is 90% by weight or more.

此外,本發明可進一步將該第三混合物或造粒後之第三混合物進行乾燥,其中該「乾燥」可採用習知的乾燥方式,而不需加以限制,較佳為熱風烘乾。本發明之方法於該步驟(3)及(4)中間進一步包含一步驟(3’),該步驟(3’)包含乾燥該第三混合物。此外,若該第三混合物要進行造粒(即步驟(3”)),則步驟(3’)之乾燥動作要接於步驟(3”)之造粒動作後實施進行。於一具體實施例中,該乾燥之溫度範圍為40℃至60℃。於另一具體實施例中,乾燥後的該第三混合物之含水率低於20%以下。於一較佳具體實施例中,乾燥後的該第三混合物之含水率低於15%以下。於一更佳具體實施例中,乾燥後的該第三混合物之含水率低於10%以下。 Further, the present invention may further dry the third mixture or the third mixture after granulation, wherein the "drying" may be carried out by a conventional drying method without limitation, and is preferably hot air drying. The method of the present invention further comprises a step (3') in the middle of the steps (3) and (4), the step (3') comprising drying the third mixture. Further, if the third mixture is to be granulated (i.e., step (3")), the drying operation of the step (3') is carried out after the granulation operation of the step (3"). In one embodiment, the drying temperature ranges from 40 °C to 60 °C. In another embodiment, the third mixture after drying has a moisture content of less than 20%. In a preferred embodiment, the third mixture after drying has a moisture content of less than 15%. In a more preferred embodiment, the third mixture after drying has a moisture content of less than 10%.

本發明將乾燥後的該第三混合物一樣進行燒結膨脹的動作,其燒結膨脹的溫度範圍為600℃至800℃;較佳地,該燒結膨脹的溫度範圍為600℃至750℃;更佳地,該燒結膨脹的溫度範圍為650℃至700℃。乾燥後的該第三混合物或造粒並乾燥後的該第三混合物進行燒結膨脹,所得為一低吸水性的多孔性材料。於一具體實施例中,該多孔性材料之吸水率為35wt%以下;較佳地,該吸水率為25wt%以下;更佳地,該吸水率為 15wt%以下。因此本發明透過是否將第三混合物進行乾燥之動作,能改變之後燒結膨脹出來的多孔性材料之吸水率。是以,本發明可以根據產品利用的需求,製造出高或低吸水率之多孔性材料。 The present invention performs the sintering expansion operation of the third mixture after drying, and the sintering expansion temperature ranges from 600 ° C to 800 ° C; preferably, the sintering expansion temperature ranges from 600 ° C to 750 ° C; more preferably The sintering expands at a temperature ranging from 650 ° C to 700 ° C. The third mixture after drying or the third mixture after granulation and drying is sintered and expanded to obtain a low water absorbing porous material. In a specific embodiment, the water absorbing material has a water absorption ratio of 35 wt% or less; preferably, the water absorption ratio is 25 wt% or less; more preferably, the water absorption ratio is 15 wt% or less. Therefore, the present invention can change the water absorption rate of the porous material which is sintered and expanded after the third mixture is dried. Therefore, the present invention can produce a porous material having a high or low water absorption rate in accordance with the demand for product utilization.

本文中的「多孔性材料」包含不限於指具有孔洞(或多孔)之陶瓷材料。因多孔性陶瓷材料具有耐高溫、穩定性高、熱傳導率低、耐沖洗、比表面積高、多孔洞、可製成閉合或相通孔洞等之優點及材質特殊性,故可發展建築用輕質骨材,隔熱性骨材、園藝保濕材、土壤保養材或水質過濾材等應用。於一具體實施例中,該多孔性材料為一骨材。由於本發明之多孔性材料因具有孔洞結構,故造成質輕,其密度小於1g/cm3;較佳地,該密度小於0.5g/cm3。於一較佳具體實施例中,該多孔性材料為一輕質骨材。 The term "porous material" as used herein is not limited to a ceramic material having pores (or porous). Because porous ceramic materials have the advantages of high temperature resistance, high stability, low thermal conductivity, high flushing resistance, high specific surface area, porous holes, closed or through holes, and material specificity, lightweight bones for construction can be developed. Materials, heat-insulating aggregates, gardening moisturizing materials, soil care materials or water filtration materials. In one embodiment, the porous material is an aggregate. Since the porous material of the present invention has a pore structure, it is light in weight and has a density of less than 1 g/cm 3 ; preferably, the density is less than 0.5 g/cm 3 . In a preferred embodiment, the porous material is a lightweight aggregate.

本發明提供一種輕質骨材,其具有一圓球狀之本體,其中該圓球狀之本體具有複數個孔洞。 The present invention provides a lightweight aggregate having a spherical body, wherein the spherical body has a plurality of holes.

於一具體實施例中,該圓球狀之本體的材質為陶瓷材料。於一較佳具體實施例中,該陶瓷材料為一白矽石。 In a specific embodiment, the spherical body is made of a ceramic material. In a preferred embodiment, the ceramic material is a chalk.

於另一具體實施例中,該圓球狀之本體的直徑小於5mm。於一較佳具體實施例中,該圓球狀之本體的直徑小於3mm。於一更佳具體實施例中,該圓球狀之本體的直徑小於1mm。 In another embodiment, the spherical body has a diameter of less than 5 mm. In a preferred embodiment, the spherical body has a diameter of less than 3 mm. In a more preferred embodiment, the spherical body has a diameter of less than 1 mm.

本發明所提供之製備多孔性材料的方法,與其他習用技術相互比較時,更具有下列之優點: The method for preparing a porous material provided by the present invention has the following advantages when compared with other conventional techniques:

(1)本發明透過將廢棄污泥(CMP污泥)以特別的製程燒結膨脹成多孔性材料(如輕質骨材),這樣再生的多孔性材料可以提供建築、土木、農業等多種用途使用,而輕質骨材最主要的應用是作為輕質混凝土的級配料,主要係提供輕質、隔音以及隔熱的效果,而含水率較高的骨材則是應用在園藝材料作為土壤保水材,更有少部分透水程度高的骨材則是作為水質淨化泥沙過濾材。輕質骨材所具有的多孔結構應在未來發展出更高附加價值之功能性材料,或結合表面處理的方式,使其表面具特殊性質,而不僅僅是作為建築材料,藉以提高輕質骨材的應用性及經濟產值,其多孔性質能否發展出氣體儲存載體、特種氣體吸附材料、特殊液體裝載容器以及土壤營養保存材等產品。故本發明之製程可達「零廢棄」、「資源再利用」及「提升再利用產品附加價值」之功效,因此本發明甚具實用價值。 (1) The present invention expands a waste sludge (CMP sludge) into a porous material (such as a lightweight aggregate) by a special process, so that the regenerated porous material can be used for various purposes such as construction, civil engineering, agriculture, and the like. The most important application of lightweight aggregates is as a graded component of lightweight concrete, mainly providing light, sound insulation and heat insulation effects, while the high water content of the aggregate is applied to horticultural materials as soil water retention material. There are also a small number of high-permeability aggregates that are used as water purification sediment filters. The porous structure of lightweight aggregates should develop higher value-added functional materials in the future, or combined with surface treatment methods to make the surface have special properties, not just as building materials, thereby improving lightweight bone. The applicability and economic output value of the material, whether its porous nature can develop gas storage carriers, special gas adsorption materials, special liquid loading containers and soil nutrient preservation materials. Therefore, the process of the present invention can achieve the effects of "zero waste", "reuse of resources" and "additional value of reused products", so the present invention has practical value.

(2)本發明於燒結膨脹前對混合物乾燥與否,可以影響所得之多孔性材料的吸水率程度。因此於相同製程上的一個步驟的改變,可以獲得不同之產品,利於製程上的效率以及產品的製造。 (2) The drying of the mixture before sintering of the present invention can affect the degree of water absorption of the resulting porous material. Therefore, a different step in the same process can obtain different products, which is beneficial to the efficiency of the process and the manufacture of the product.

(3)本發明使用高含矽量之工業副產物(CMP污泥),在小於800℃之燒結膨脹程序下可生產出輕質骨材,相較於現有其他汙泥製作輕質骨材之製程,其燒結膨脹溫度皆高於900℃,本發明之製程所使用燒結溫度較低(低於800℃)一樣可以製造出輕質骨材,故本發明能有效降低熱耗能以及減少高溫造成的環境影響。 (3) The present invention uses a high by-product industrial by-product (CMP sludge) to produce a lightweight aggregate under a sintering expansion procedure of less than 800 ° C, and to produce a lightweight aggregate compared to other existing sludges. The process has a sintering expansion temperature higher than 900 ° C. The process of the invention uses a lower sintering temperature (less than 800 ° C) to produce a lightweight aggregate, so the invention can effectively reduce heat energy consumption and reduce high temperature. Environmental impact.

10‧‧‧輕質骨材 10‧‧‧Light aggregate

100‧‧‧圓球狀之本體 100‧‧‧ spherical body

200‧‧‧孔洞 200‧‧‧ holes

圖1為以化學機械研磨製程(Chemical-Mechanical Polishing;CMP)汙泥製作輕質骨材之流程。 Figure 1 shows the process of making lightweight aggregates using Chemical-Mechanical Polishing (CMP) sludge.

圖2為擠出造粒之粒體形狀。 Figure 2 shows the shape of the granules by extrusion granulation.

圖3為以CMP汙泥樣本1所製得之低水率的多孔性輕質骨材。 Fig. 3 is a low-water ratio porous lightweight aggregate obtained by CMP sludge sample 1.

圖4為以CMP汙泥樣本2所製得之高水率的多孔性輕質骨材。 Figure 4 is a high water rate porous lightweight aggregate obtained from CMP sludge sample 2.

圖5為以CMP汙泥樣本3所製得之低水率的多孔性輕質骨材。 Fig. 5 is a low-water ratio porous lightweight aggregate obtained by using CMP sludge sample 3.

圖6為本發明之輕質骨材的多孔性結構。 Figure 6 is a view showing the porous structure of the lightweight aggregate of the present invention.

圖7為本發明之輕質骨材的結構。 Figure 7 is a view showing the structure of the lightweight aggregate of the present invention.

本發明包括但不限於上述與下開之說明。實施方式則如下範例所示。 The invention includes, but is not limited to, the description above and below. The embodiment is shown in the following example.

A.再生輕質骨材之製作流程 A. Production process of recycled lightweight aggregate

1.半導體製程中化學機械研磨所產生之污泥的成分鑑定 1. Identification of the components of sludge produced by chemical mechanical polishing in a semiconductor process

半導體廠將化學機械研磨製程(Chemical-Mechanical Polishing;CMP)應用於晶圓製造程序中時,其會產生大量的CMP汙泥。本發明對三個CMP汙泥樣本進行X光螢光分析儀(X-ray Fluorescence Spectrometer;XRF)檢測,其成分分析檢測數據如表一所示,從表一之結果可知各個CMP汙泥樣本中二氧化矽(SiO2)含量達70%以上,故可進行後續製程。 When a semiconductor factory applies Chemical-Mechanical Polishing (CMP) to a wafer fabrication process, it produces a large amount of CMP sludge. The three CMP sludge samples are subjected to X-ray Fluorescence Spectrometer (XRF) detection, and the component analysis and detection data are shown in Table 1. From the results of Table 1, the CMP sludge samples are known. The content of cerium oxide (SiO 2 ) is over 70%, so subsequent processes can be carried out.

2.製備流程 2. Preparation process

CMP汙泥製作輕質骨材之流程如圖1所示,其步驟順序如下: The process of making lightweight aggregates from CMP sludge is shown in Figure 1. The sequence of steps is as follows:

(1)乾燥:CMP汙泥會因CMP製程而含有大量的水份(含水率約55至70%),因此可以透過熱風乾燥旋轉窯或熱風乾燥機烘乾CMP汙泥,使之乾燥,將CMP汙泥的水份去除變成含水率小於1%之CMP汙泥塊體或 CMP汙泥餅。 (1) Drying: CMP sludge will contain a large amount of water (water content of about 55 to 70%) due to the CMP process. Therefore, the CMP sludge can be dried by a hot air drying rotary kiln or a hot air dryer to dry it. The moisture removal of the CMP sludge becomes a CMP sludge block or CMP sludge cake having a moisture content of less than 1%.

(2)混合及研磨:將一黏土類礦物(如高嶺土)及一發泡劑(如碳酸鈉或碳酸鈣)加入進乾燥後的CMP汙泥塊體或CMP汙泥餅中混合以調整其化學組成,並經過球磨混合成一粉體混合物;而混合時,是先將重量百分比為85%至95%之CMP汙泥與重量百分比5%至15%之黏土類礦物混合,得一混合物,再添加發泡劑,其添加量為該混合物之總重量的0.5至8%。 (2) Mixing and grinding: a clay mineral (such as kaolin) and a foaming agent (such as sodium carbonate or calcium carbonate) are added to the dried CMP sludge block or CMP sludge cake to adjust its chemistry. Composition, and ball milled to form a powder mixture; and mixing, firstly, 85% to 95% by weight of CMP sludge is mixed with 5% to 15% by weight of clay minerals to obtain a mixture, and then added A blowing agent is added in an amount of from 0.5 to 8% by weight based on the total weight of the mixture.

(3)攪拌:該粉體混合物與一黏結劑混合,該黏結劑會使該粉體混合物黏結成一塊,經過攪拌會成一膏狀物,如麵團狀。該黏結劑包含一鹼金屬或一鹼土金屬化合物溶液;以鹼金屬化合物溶液為例,混合時,該粉體混合物與該鹼金屬化合物溶液混合之重量百分比比例為鹼金屬化合物溶液占18%至60%。於本發明中,該鹼金屬化合物溶液選用氫氧化鈉溶液。 (3) Stirring: The powder mixture is mixed with a binder which binds the powder mixture into a piece which, when stirred, forms a paste, such as a dough. The binder comprises an alkali metal or alkaline earth metal compound solution; in the case of an alkali metal compound solution, when mixed, the powder mixture is mixed with the alkali metal compound solution in a weight percentage ratio of an alkali metal compound solution of 18% to 60%. %. In the present invention, the alkali metal compound solution is selected from a sodium hydroxide solution.

(4)造粒:將膏狀物透過擠出成型機擠出條狀物並切粒成目標大小進行造粒,得一粒體骨材。故使用者可以依據最終成品的尺寸大小需求進行造粒,例如切成粒徑小於3至5mm之顆粒。 (4) Granulation: The paste is extruded through an extrusion molding machine and granulated into a target size for granulation to obtain a granulated aggregate. Therefore, the user can granulate according to the size requirement of the final product, for example, dicing into particles having a particle diameter of less than 3 to 5 mm.

(5)燒結膨脹:(i)將切粒之粒體骨材,於未經乾燥程序下,直接在旋窯中進行燒結膨脹程序,其燒結膨脹之溫度為400至700℃,則形成高吸水率 (吸水率為70wt%以上)之多孔性輕質骨材;或(ii)將該切粒之粒體骨材再進行一次乾燥程序,如於熱風下(40至60℃)乾燥至含水率小於15%之粒體骨材,乾燥後再於旋窯進行燒結膨脹,其燒結膨脹之溫度為600至800℃,則獲得低吸水率(吸水率為35wt%以下)之多孔性輕質骨材。 (5) Sintering expansion: (i) The granulated aggregates of the pellets are directly subjected to a sintering expansion process in a rotary kiln without drying, and the sintering expansion temperature is 400 to 700 ° C, thereby forming a high water absorption. a porous lightweight aggregate having a rate (water absorption of 70% by weight or more); or (ii) drying the granulated aggregate of the granules again, such as drying under hot air (40 to 60 ° C) to moisture content Less than 15% of the granule aggregate, dried and then sintered and expanded in a rotary kiln, and the sintering expansion temperature is 600 to 800 ° C, thereby obtaining a porous lightweight aggregate having a low water absorption rate (water absorption ratio of 35 wt% or less) .

B.性質測試方法 B. Nature test method

透過上述製程所獲得之產品之吸水率及密度量測方式為:將產品於空氣中先行量測其重量(Wa),置於水中24小時後,量測水中的重量(Ww),取出產品將其表面擦拭達表面乾淨並稱量其重量(Wb)。因此,吸水率的算法為(以重量百分率表示):吸水率:[(Wb-Wa)/Wa]x100% The water absorption rate and density measurement method of the product obtained through the above process is as follows: the product is first measured in the air (Wa), and after being placed in water for 24 hours, the weight (Ww) in the water is measured, and the product is taken out. The surface is wiped to a clean surface and its weight (Wb) is weighed. Therefore, the algorithm for water absorption is (in weight percent): water absorption: [(Wb-Wa)/Wa] x 100%

密度的算法為(以g/cm3表示):密度:Wa/[(Wb-Ww)/1(水的密度)] The algorithm for density is (in g/cm 3 ): density: Wa / [(Wb - Ww) / 1 (density of water)]

因量測介質為水,其密度是1(g/cm3),故利用重量回推其體積和密度。 Since the measurement medium is water and its density is 1 (g/cm 3 ), its volume and density are pushed back by weight.

此外,本發明利用承壓筒,以測定顆粒的平均相對抗壓強度指標,作為評定粗顆粒品質之用。粗顆粒筒壓強度試驗法,其步驟包含:(1)篩取5L之3至5mm粒徑的樣品;(2)用承壓筒(帶筒底)裝樣品,分別測定3次鬆散料重,取其算數平均值;(3)按上述樣品量稱取樣品,分3次裝入承壓筒,每次均先以搗桿在表面均勻搗實25次,並且用木錘沿筒壁 四周分四點輕敲3至5次,然後裝上導向筒和沖壓模,檢查沖壓模的下刻度紋是否與導向筒的上緣重合,如不重合,再輕敲筒壁四周,直至完全重合為止;及(4)把承壓筒放在壓力機的下壓板上,以每秒約30至50kgf的均勻速度加荷,當沖壓模壓入深度為20mm時,記下壓力值。顆粒的筒壓強度之計算為:R=P/F Further, the present invention utilizes a pressure cylinder to measure the average relative compressive strength index of the particles as an evaluation of the quality of the coarse particles. The coarse particle barrel compressive strength test method comprises the steps of: (1) screening 5 L of a sample having a particle size of 3 to 5 mm; (2) loading a sample with a pressure tube (with a bottom), and measuring the loose bulk weight three times, respectively. Take the arithmetic mean; (3) Weigh the sample according to the above sample volume, and put it into the pressure cylinder 3 times, each time to be evenly tamped on the surface with a mast for 25 times, and use a wooden hammer to divide the wall around the wall. Tap three to five times at four points, then install the guiding cylinder and the stamping die to check whether the lower scale of the stamping die coincides with the upper edge of the guiding cylinder. If it does not overlap, tap the wall around the cylinder until it is completely coincident; And (4) placing the pressure cylinder on the lower pressure plate of the press, and loading at a uniform speed of about 30 to 50 kgf per second. When the press mold is pressed to a depth of 20 mm, the pressure value is recorded. The calculation of the compressive strength of the pellet is: R = P / F

R:輕質骨材的筒壓強度(kg/cm2),計算精確至1kg/cm2;P:壓入深度為20mm時的壓力值(kg);及F:承壓面積(即沖壓模面積F=100cm2)。 R: the cylinder strength (kg/cm 2 ) of the lightweight aggregate, calculated to the accuracy of 1 kg/cm 2 ; P: the pressure value (kg) when the penetration depth is 20 mm; and F: the pressure-bearing area (ie, the stamping die) Area F = 100 cm 2 ).

C.產品製造 C. Product manufacturing

產品1(低吸水率型) Product 1 (low water absorption type)

經過乾燥後去除CMP汙泥樣本1中約60%的水分,再於95wt%乾燥後的CMP汙泥樣本1添加5wt%的高嶺土且額外添加0.5wt%的過碳酸鈉後,以球磨機進行均勻研磨形成一骨材粉體,其中該骨材粉體係指可通過100號篩網之粉末。再以5N莫耳濃度(約20wt%)的氫氧化鈉與該骨材粉體混合攪拌直到適合黏度後,進行擠出造粒,粒體大小為3至5mm(如圖2)。造粒後之粒體再次乾燥(如於40至60℃熱風下乾燥,將粒體的含水率降至15%以下),再於旋窯中進行680℃之燒結膨脹程序,獲得多孔性輕質骨材(如圖3),該骨材之特性為體密度為0.62g/cm3,堆積密度為0.36g/cm3,吸水率為12wt%,抗壓強度為5.34MPa(約54.5kg/cm2)。 After drying, about 60% of the moisture in the CMP sludge sample 1 was removed, and then 5 wt% of kaolin was added to the 95 wt% dried CMP sludge sample 1 and 0.5 wt% of sodium percarbonate was additionally added, followed by uniform grinding by a ball mill. An aggregate of bone material is formed, wherein the aggregate powder system refers to a powder that can pass through a No. 100 sieve. Further, 5 N molar concentration (about 20% by weight) of sodium hydroxide was mixed with the aggregate powder until the viscosity was suitable, and extrusion granulation was carried out, and the granule size was 3 to 5 mm (Fig. 2). After granulation, the granules are dried again (for example, drying at 40 to 60 ° C under hot air to reduce the water content of the granules to less than 15%), and then performing a sintering expansion process at 680 ° C in a rotary kiln to obtain a porous lightweight material. The aggregate (Fig. 3) has a bulk density of 0.62 g/cm 3 , a bulk density of 0.36 g/cm 3 , a water absorption of 12 wt%, and a compressive strength of 5.34 MPa (about 54.5 kg/cm). 2 ).

產品2(高吸水率型) Product 2 (high water absorption type)

經過乾燥後,去除CMP汙泥樣本2約60%水分,將92wt%乾燥後的CMP汙泥樣本2經過添加8wt%的高嶺土且額外添加2wt%的碳酸鈣後,以球磨機均勻研磨形成骨材粉體,其中該骨材粉體係指可通過100號篩之粉末。再以5N莫耳濃度(約20wt%)的氫氧化鈉與該骨材粉體混合攪拌直到適合黏度後,進行擠出造粒,粒體大小為3至5mm。造粒後之粒體直接於旋窯中進行550℃燒結膨脹程序,獲得一多孔性輕質骨材(如圖4),其特性為體密度0.37g/cm3,吸水率為92wt%,抗壓強度為1.23MPa(約12.5kg/cm2)。 After drying, the CMP sludge sample 2 is removed by about 60% moisture, and 92% by weight of the dried CMP sludge sample 2 is added to 8 wt% of kaolin and an additional 2 wt% of calcium carbonate is added, and then uniformly ground by a ball mill to form an aggregate powder. Body, wherein the aggregate powder system refers to a powder that can pass through a No. 100 sieve. Further, 5 N molar concentration (about 20% by weight) of sodium hydroxide was mixed with the aggregate powder until the viscosity was suitable, and extrusion granulation was carried out, and the granule size was 3 to 5 mm. The granulated granules were directly subjected to a 550 ° C sintering expansion procedure in a rotary kiln to obtain a porous lightweight aggregate (Fig. 4) having a bulk density of 0.37 g/cm 3 and a water absorption of 92 wt%. The compressive strength was 1.23 MPa (about 12.5 kg/cm 2 ).

產品3(低吸水率型) Product 3 (low water absorption type)

使用CMP汙泥樣本3作為原料使用時,先乾燥去除約60%水分後,添加10wt%的高嶺土於90wt%乾燥後的CMP汙泥樣本3中且額外添加2wt%的碳酸氫鈉後,以球磨機均勻研磨形成骨材粉體,其中該骨材粉體係指可通過100號篩之粉末。再以14N莫耳濃度(約55wt%)的氫氧化鈉與該骨材粉體混合攪拌直到適合黏度後,進行擠出造粒,粒體大小為3至5mm。造粒後之粒體再次乾燥(如於40至60℃熱風下乾燥,將粒體的含水率降至15%以下),再於旋窯中進行680℃燒結膨脹程序,獲得一多孔性輕質骨材(如圖5),其體密度為0.43g/cm3,吸水率為10wt%。 When using CMP sludge sample 3 as a raw material, after drying and removing about 60% of water, adding 10 wt% of kaolin in 90 wt% of dried CMP sludge sample 3 and additionally adding 2 wt% of sodium hydrogencarbonate, and then using a ball mill The aggregate is uniformly ground to form an aggregate powder, wherein the aggregate powder system refers to a powder that can pass through a No. 100 sieve. Further, 14 N molar concentration (about 55 wt%) of sodium hydroxide was mixed with the aggregate powder until the viscosity was suitable, and extrusion granulation was carried out, and the granule size was 3 to 5 mm. After granulation, the granules are dried again (for example, drying at 40 to 60 ° C under hot air to reduce the water content of the granules to less than 15%), and then performing a 680 ° C sintering expansion procedure in a rotary kiln to obtain a porous light. The material (Fig. 5) has a bulk density of 0.43 g/cm 3 and a water absorption of 10 wt%.

圖6為上述多孔性輕質骨材的產品之多孔性結構,因具有多孔性結構故造成骨材能質輕,其密度小於1g/cm3Fig. 6 is a view showing the porous structure of the product of the above porous lightweight aggregate, which has a porous structure and is light in energy, and has a density of less than 1 g/cm 3 .

表二為三個CMP汙泥樣本所製得的多孔性輕質骨材之性質比較。 Table 2 compares the properties of porous lightweight aggregates made from three CMP sludge samples.

圖7為本發明之輕質骨材的結構,該輕質骨材10具有一圓球狀之本體100,其中該圓球狀之本體具有複數個孔洞200。該圓球狀之本體的材質為陶瓷材料,進一步來說,該陶瓷材料之組成為白矽石礦物。此外,該圓球狀之本體的直徑小於5mm。 7 is a structure of a lightweight aggregate of the present invention, the lightweight aggregate 10 having a spherical body 100, wherein the spherical body has a plurality of holes 200. The material of the spherical body is a ceramic material, and further, the composition of the ceramic material is a chalk mineral. Further, the spherical body has a diameter of less than 5 mm.

本發明適當的描述可以在本文未具體公開的元素或限制下實施。已被用作描述的術語並不是限制。在使用這些術語和除此之外的任何等同物的表達和描述是沒有差別的,但應當認識到本發明內的權利是可能修改的。因此,雖然本發明已說明實施例和其他情況,本文中所公開的內容可以被本領域的技術人員進行修飾和變化,並且這樣的修改和變化被認為是在本發明的權利範圍之內。 Suitable descriptions of the invention may be implemented in elements or limitations not specifically disclosed herein. The terminology that has been used for description is not limiting. There is no difference in the expression and description of the use of these terms and any equivalents, but it is to be understood that the scope of the invention may be modified. Therefore, the present invention has been described with reference to the embodiments and other aspects, and the modifications and variations of the present invention are considered to be within the scope of the present invention.

Claims (15)

一種製備多孔性材料的方法,其包含:(1)提供一乾燥的半導體製程中化學機械研磨所產生之污泥;(2)將該乾燥的半導體製程中化學機械研磨所產生之污泥及一黏土礦物混合,得一第一混合物,再添加一發泡劑於該第一混合物中,並研磨成粉體,得一第二混合物;(3)將該第二混合物與一黏結劑混合,得一第三混合物;以及(4)燒結膨脹該第三混合物,得一多孔性材料。  A method for preparing a porous material, comprising: (1) providing sludge produced by chemical mechanical polishing in a dry semiconductor process; (2) sludge produced by chemical mechanical polishing in the dried semiconductor process and Mixing the clay mineral to obtain a first mixture, adding a blowing agent to the first mixture, and grinding into a powder to obtain a second mixture; (3) mixing the second mixture with a binder to obtain a third mixture; and (4) sintering to expand the third mixture to obtain a porous material.   如申請專利範圍第1項所述之方法,其中該乾燥的半導體製程中化學機械研磨所產生之污泥之含水率低於1%。  The method of claim 1, wherein the sludge produced by the chemical mechanical polishing in the dry semiconductor process has a moisture content of less than 1%.   如申請專利範圍第1項所述之方法,其中該乾燥的半導體製程中化學機械研磨所產生之污泥占該第一混合物的重量百分比為85%至95%。  The method of claim 1, wherein the chemical mechanical grinding in the dry semiconductor process comprises from 85% to 95% by weight of the first mixture.   如申請專利範圍第1項所述之方法,其中該黏土礦物占該第一混合物的重量百分比為5%至15%。  The method of claim 1, wherein the clay mineral comprises from 5% to 15% by weight of the first mixture.   如申請專利範圍第1項所述之方法,其中該發泡劑的添加量為該第一混合物之總重量的0.5%至8%。  The method of claim 1, wherein the blowing agent is added in an amount of from 0.5% to 8% by weight based on the total weight of the first mixture.   如申請專利範圍第1項所述之方法,其中該黏結劑占該第三混合物的重量百分比為18%至60%  The method of claim 1, wherein the binder accounts for 18% to 60% by weight of the third mixture.   如申請專利範圍第1項所述之方法,該黏結劑包含一鹼金屬化合物溶液 或一鹼土金屬化合物溶液。  The method of claim 1, wherein the binder comprises an alkali metal compound solution or an alkaline earth metal compound solution.   如申請專利範圍第7項所述之方法,其中該鹼金屬化合物溶液為一鹼金屬氫氧化物溶液。  The method of claim 7, wherein the alkali metal compound solution is an alkali metal hydroxide solution.   如申請專利範圍第8項所述之方法,其中該鹼金屬氫氧化物溶液為一氫氧化鈉溶液。  The method of claim 8, wherein the alkali metal hydroxide solution is a sodium hydroxide solution.   如申請專利範圍第1項所述之方法,其中該燒結膨脹的溫度範圍為400℃至800℃。  The method of claim 1, wherein the sintering expands at a temperature in the range of 400 ° C to 800 ° C.   如申請專利範圍第1項所述之方法,其中該多孔性材料之吸水率為70wt%以上。  The method of claim 1, wherein the porous material has a water absorption of 70% by weight or more.   如申請專利範圍第1項所述之方法,其中該步驟(3)及(4)中間進一步包含一步驟(3’),該步驟(3’)包含乾燥該第三混合物。  The method of claim 1, wherein the step (3) and (4) further comprises a step (3'), the step (3') comprising drying the third mixture.   如申請專利範圍第12項所述之方法,其中乾燥後的該第三混合物之含水率低於15%。  The method of claim 12, wherein the third mixture after drying has a moisture content of less than 15%.   如申請專利範圍第12項所述之方法,其中該燒結的溫度範圍為600℃至800℃。  The method of claim 12, wherein the sintering temperature ranges from 600 ° C to 800 ° C.   如申請專利範圍第12項所述之方法,其中該多孔性材料之吸水率為35wt%以下。  The method of claim 12, wherein the porous material has a water absorption of 35 wt% or less.  
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