200827457 九、發明說明： 【發明所屬之技術領域】 本發明係關於一種分離鋼中介在物的方法，詳言之，係 關於一種增加一還原步驟之分離鋼中介在物的方法。 【先前技術】 煉鋼過程中，為了脫除多餘的氧，通常會加入親和力比 鐵大元素。以含鋁量〇·〇2%以上的低碳高清淨度鋼種（例 如：馬口鐵、汽車用鋼和深沖用低碳冷軋鋼片等一般鋁脫 氧鋼）的製程為例，會在轉爐後的精煉步驟裡，添加鋁來 進行脫氧作業。一般而言，鋁是純淨鋼中常用而且是非常 強的脫氧劑’當其加進鋼液後會和鋼液中的氧產生反應， 开> 成微細顆粒的固相氧化銘介在物（inclusi〇n)，較大型的 介在物（顆粒尺寸大於50 μπ!)會上浮而吸附於渣中，但是 小型的介在物（顆粒尺寸數十μηι以下）則會殘留在鋼中，形 成惱人的缺陷問題。 介在物以來源分類可分為：外來介在物及内生介在物。 δ亥外來介在物之來源係為耐火材或炼潰，其外形不規則， 尺寸較大和分佈不均勻。該内生介在物係脫氧或凝固過程 生成，其顆粒較小，分佈均勻。 介在物以化學成分分類可分為：氧化物介在物、硫化物 介在物及氮化物介在物。氧化物介在物包括：（1)簡單氧化 物：FeO、MnO、Si02、Α12〇3 ; (2)複雜氧化物：FeO · Al2〇3、MnO · Al2〇3、Mgo · Al2〇3 ; (3)矽酸鹽：2FeO · Si02、2MnO · Si02、3MnO · Al2〇3 · 2Si02。硫化物介在 116092.doc 200827457 物包括·· FeS、MnS、（Fe · Mn)S、CaS。氮化物介在物包 括·· AIN、TiN、BN、ZrN。 由於鋼中介在物會影響鋼材的機械性及加工性，因此需 要從鋼中分離出該介在物加以分析。 習知從鋼中分離該介在物的方法有二：電解法（sli_BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for separating steel intermediaries, and more particularly to a method for increasing the separation of steel in a reduction step. [Prior Art] In the steelmaking process, in order to remove excess oxygen, it is usually added to an element with a higher affinity than iron. For example, the process of low-carbon high-definition steel grades with aluminum content of 〇·〇2% or more (for example, tinplate iron, automotive steel, and general-purpose aluminum deoxidized steel for deep-drawn cold-rolled steel sheets) will be used after the converter. In the refining step, aluminum is added for deoxidation. In general, aluminum is a commonly used and very strong deoxidizer in pure steel. When it is added to molten steel, it reacts with oxygen in the molten steel. It is a solid phase oxidation of fine particles. 〇n), the larger type of intervening material (particle size greater than 50 μπ!) will float up and adsorb in the slag, but the small intervening material (particle size below tens μηι) will remain in the steel, forming an annoying defect problem. . The mediation can be divided into: foreign mediators and endogenous mediators. The source of the material is refractory material or refining, and its shape is irregular, the size is large and the distribution is uneven. The endogenous medium is formed during deoxidation or solidification of the system, and the particles are small and evenly distributed. The substances can be classified into chemical mediators, sulfide mediators, and nitride mediators. The oxide intermediaries include: (1) simple oxides: FeO, MnO, SiO 2 , Α12〇3; (2) complex oxides: FeO · Al2〇3, MnO · Al2〇3, Mgo · Al2〇3; ) Citrate: 2FeO · SiO 2 , 2MnO · SiO 2 , 3MnO · Al 2 〇 3 · 2Si02. Sulfide is contained in 116092.doc 200827457. It includes FeS, MnS, (Fe · Mn)S, and CaS. Nitride intercalates include AIN, TiN, BN, and ZrN. Since the steel intermediaries affect the mechanical and processability of the steel, it is necessary to separate the intervening material from the steel for analysis. There are two ways to separate the intervening material from steel: electrolysis (sli_
Method)及酸溶法。電解法係利用電位電解方式溶解金屬 鐵，以過濾方式將介在物分離，再藉由儀器定量分析該介 在物的成分及含量。此種方法之缺點為會產生大量淤泥， 不易過濾，最終所得到的介在物顆粒尺寸以大於5〇 pm居 夕，不此應用於顆粒尺寸小於2〇 μιη的小型介在物。另 外，酸溶法係利用低溫弱酸將鋼材樣品溶解，再以過濾方 弋刀離”在物此種方法的缺點為會有鐵基質溶解不完全 的門題因此在過濾時必須多次使用大量的溫酸液來沖 洗，如此會產生大量酸液。 因此，有必要提供一種創新且具進步性的分離鋼中介在 物的方法，以解決上述問題。 【發明内容】Method) and acid dissolution method. In the electrolysis method, the metal iron is dissolved by the potential electrolysis method, the intervening substance is separated by filtration, and the composition and content of the medium are quantitatively analyzed by an instrument. The disadvantage of this method is that a large amount of sludge is generated, which is difficult to filter, and the resulting intermediate particle size is greater than 5 pm, and is not applied to small intermediaries having a particle size of less than 2 Å μηη. In addition, the acid-soluble method uses a low-temperature weak acid to dissolve the steel sample, and then uses a filter to remove the knives. The disadvantage of this method is that there is a problem that the iron matrix is incompletely dissolved. Therefore, it is necessary to use a large number of times during filtration. Washing with warm acid solution will produce a large amount of acid solution. Therefore, it is necessary to provide an innovative and progressive method for separating steel intermediates to solve the above problems.
本發明之主要目的在於提供一種分離鋼中介在物的方 介在物。藉此， · (a)提供一鋼樣品；（b)溶解該鋼樣 一溶液；（c)過濾及烘乾該第一溶液，以取 (d)對該第一粉末進行還原反應；（e)溶解 粉末，以形成一第二溶液；及（f)過濾及烘 以取得一第二粉末，該第二粉束係包含該 正個分離鋼中介在物所花費的時間縮短， 116092.doc 200827457 與t知方法相比’本發明可以節省一半的時間。此外，利 用本發明之方法所分離出之介在物之顆粒尺寸可以小到 0.5 μηι’因此可以應用到顆粒尺寸小於2〇 的小型介在 物。 【實施方式】 參考圖1，顯示本發明分離鋼中介在物的方法之較佳實 施例之流程圖。本發明所分離之介在物之種類包括氧化物 介在物、硫化物介在物及氮化物介在物。氧化物介在物包 括：⑴簡單氧化物·· FeO、MnO、Si02、Al2〇3 ; (2)複雜 乳化物· FeO · Al2〇3、MnO · Al2〇3、MgO · Al2〇3 ; (3)石夕 酸鹽：2FeO · Si02、2MnO · Si02、3MnO · Al2〇3 · 2Si〇2。硫化物介在物包括·· FeS、MnS、（Fe · Mn)S、 CaS。氮化物介在物包括：AIN、TiN、BN、ZrN。 本發明之該方法包括以下步驟。步驟S101係提供一鋼樣 品’亦即從一鋼材中取適量的鋼樣品。在本實施例中，該 鋼樣品之取樣數量約200克。在本實施例中，該鋼樣品係 為鋁脫氧鋼，其可以是馬口鐵、1〇〇8 A鋼、軸承鋼、低碳 鋼或熱浸鍍辞（GA)鋼。 步驟S 102係利用一酸洗液酸洗該鋼樣品之表面，以去除 該鋼樣品表面上之油脂及金屬屑。該酸洗液可以是鹽酸、 硝酸或硫酸等。在本實施例中，該酸洗液之濃度係為20重 量百分比（wt%)，體積係為4公升，溫度係為55°C。在本實 施例中，係利用鹽酸酸洗該鋼樣品之表面。 步驟S 1 03係利用一第一酸液將該鋼樣品溶解，以形成一 116092.doc 200827457 第一溶液。該第一酸液可以是鹽酸、硝酸或硫酸等，其濃 度為10〜30重量百分比（wt%)，其體積為每克鋼樣品對應 1〜3宅升之該第一酸液，其溫度為50〜90°C。要注意的是， 该第一酸液之種類係對應該鋼樣品或是該介在物之材質， 亦即該第一酸液之選擇標準為可以將鋼樣品溶解但是不能 將該介在物溶解之酸液。 在本實施例中，係在5公升燒杯中加入硝酸1〇〇〇 cc及水 3000 cc ’再將該2〇〇克鋼樣品置入該燒杯中。接著，攪拌 及加熱至5 5。(： ’使該鋼樣品完全溶解，以形成一第一溶 液。 步驟S 104係過濾及烘乾該第一溶液，以取得一第一粉 末。該過濾步驟係利用一濾紙進行過濾，其中該濾紙之孔 径（Pore)係為2〜7 μπι，較佳為4〜5 μπι。由於在過渡過程 中，該濾紙之上表面上會形成一濾餅，該濾餅之孔徑會小 於該濾紙之孔徑，因此即使顆粒尺寸小於1 μηι的介在物也 會殘留在該濾餅中。在本實施例中，係先冷卻該第一溶液 後，再利用孔徑為4〜5 μηι之濾紙過濾該第一溶液，再將該 濾紙上之殘留物放至一高溫爐中烘乾以完全灰化約8〇〇 °C，以取得一第一粉末，第一粉末係包含鐵基質物質及氧 化铭介在物。 步驟S105係對該第一粉末進行還原反應。該還原反應可 以利用許多方式達成，舉例而言，可以將該第一粉末置於 一還原性氣體（例如氫氣）中，反應溫度為6〇〇〜700°C，以 對該第一粉末進行還原反應，使得該第一粉末中鐵基質物 116092.doc -9- 200827457 貝還原成金屬鐵。在本實施例中，係將該第一粉末置於— 官狀爐’該管狀爐内含氫氣且溫度為650°C，以對該第一 粉末進行還原反應，使得該第一粉末中鐵基質物質還原成 金屬鐵。 步驟S106係利用一第二酸液將該還原後之第一粉末溶 解’以形成一第二溶液。該第二酸液可以是鹽酸、硝酸或 硫酸等，該第二酸液可以與該第一酸液相同或不相同，但 是其體積可以少許多。在本實施例中，該第二酸液係為稀 鹽酸’其濃度係為1 8重量百分比（wt%)、體積係為50 cc， 溫度係為25°C，其可以將該金屬鐵溶解，以形成一第二溶 液0 步驟S107係過濾及烘乾該第二溶液，以取得一第二粉 末。本過濾步驟與該步驟S 104之過濾步驟一樣，皆利用一 濾紙進行過濾，其中該濾紙之孔徑（Pore)係為2〜7 μιη，較 佳為4〜5 μιη。本步驟所使用之濾紙可以與步驟sl〇4相同， 然而可以理解的是，本步驟之濾紙可以與步驟S104不同。 在本實施例中，係先冷卻該第二溶液後，再利用孔徑為 4〜5 μιη之濾紙過濾該第二溶液，再將該濾紙上之殘留物放 至該高溫爐中烘乾以完全灰化約8〇〇°C，以取得一第二粉 末，第二粉末係包含該氧化鋁介在物，且該氧化鋁介在物 之顆粒尺寸係大於0.5 μιη以上。 接著，如果需要的話，可以再藉由儀器定量分析該氧化 紹介在物的成分及含量。 本發明之優點為整個分離鋼中介在物所花費的時間縮 116092.doc -10- 200827457 短’與習知方法相比，太 本毛明可以節省一半的 外，利用本發明之方法所分離 、s。此 出之在物之顆粒尺寸可以 小到〇·5 μηι，因此可以肩 丁了以 介在物。 應用到顆粒尺寸小於〜的小型SUMMARY OF THE INVENTION A primary object of the present invention is to provide a means for separating steel intermediaries. Thereby, (a) providing a steel sample; (b) dissolving the steel sample-solution; (c) filtering and drying the first solution to obtain (d) a reduction reaction of the first powder; Dissolving the powder to form a second solution; and (f) filtering and baking to obtain a second powder, the second powder bundle comprising the time taken for the positive separation steel to be interposed, 116092.doc 200827457 Compared with the t-knowledge method, the present invention can save half of the time. Further, the particle size of the intervening substance separated by the method of the present invention can be as small as 0.5 μηι', and thus can be applied to a small-sized medium having a particle size of less than 2 Å. [Embodiment] Referring to Figure 1, there is shown a flow chart of a preferred embodiment of the method of separating steel intermediaries of the present invention. The types of intervening materials isolated in the present invention include oxide mediators, sulfide mediators, and nitride mediators. The oxide intermediaries include: (1) simple oxides · FeO, MnO, SiO 2 , Al 2 〇 3 ; (2) complex emulsions · FeO · Al2〇3, MnO · Al2〇3, MgO · Al2〇3; (3) Oleic acid salt: 2FeO · SiO 2 , 2MnO · Si02, 3MnO · Al2〇3 · 2Si〇2. Sulfide mediators include FeS, MnS, (Fe·Mn)S, and CaS. The nitride intervening material includes: AIN, TiN, BN, ZrN. The method of the invention comprises the following steps. In step S101, a steel sample is provided, i.e., an appropriate amount of steel sample is taken from a steel material. In this embodiment, the steel sample is sampled in an amount of about 200 grams. In the present embodiment, the steel sample is aluminum deoxidized steel, which may be tinplate, 1 〇〇 8 A steel, bearing steel, low carbon steel or hot dip galvanized (GA) steel. Step S102 is to pickle the surface of the steel sample with an acid pickling solution to remove grease and metal shavings on the surface of the steel sample. The pickling liquid may be hydrochloric acid, nitric acid or sulfuric acid or the like. In the present embodiment, the concentration of the pickling liquid was 20 weight percent (wt%), the volume was 4 liters, and the temperature was 55 °C. In this embodiment, the surface of the steel sample is pickled with hydrochloric acid. Step S1 03 dissolves the steel sample with a first acid solution to form a first solution of 116092.doc 200827457. The first acid solution may be hydrochloric acid, nitric acid or sulfuric acid, etc., and the concentration thereof is 10 to 30 weight percent (wt%), and the volume thereof is 1 to 3 liters of the first acid solution per gram of the steel sample, and the temperature thereof is 50~90 °C. It should be noted that the type of the first acid liquid corresponds to the material of the steel sample or the material of the medium, that is, the selection criterion of the first acid liquid is an acid which can dissolve the steel sample but cannot dissolve the medium. liquid. In this example, a 1 gram of nitric acid and 3000 cc of water were added to a 5 liter beaker and the 2 gram steel sample was placed in the beaker. Then, stir and heat to 5 5 . (: 'The steel sample is completely dissolved to form a first solution. Step S104 is to filter and dry the first solution to obtain a first powder. The filtering step is performed by using a filter paper, wherein the filter paper The pore diameter (Pore) is 2 to 7 μπι, preferably 4 to 5 μπι. Since a filter cake is formed on the upper surface of the filter paper during the transition, the pore size of the filter cake is smaller than the pore diameter of the filter paper. Therefore, even if the mediator having a particle size of less than 1 μm is left in the filter cake, in the present embodiment, after the first solution is cooled, the first solution is filtered using a filter paper having a pore diameter of 4 to 5 μm. Then, the residue on the filter paper is placed in a high temperature furnace to be dried to completely ash about 8 ° C to obtain a first powder, and the first powder contains an iron matrix substance and an oxidation medium. Step S105 The first powder is subjected to a reduction reaction. The reduction reaction can be achieved in many ways. For example, the first powder can be placed in a reducing gas (for example, hydrogen) at a reaction temperature of 6 〇〇 to 700 °. C, to the right The first powder is subjected to a reduction reaction such that the iron matrix 116092.doc -9-200827457 is reduced to metallic iron in the first powder. In the present embodiment, the first powder is placed in the official furnace. The furnace contains hydrogen gas and the temperature is 650 ° C to reduce the first powder in the first powder to reduce the iron matrix material to metal iron. Step S106 uses a second acid solution to reduce the first A powder is dissolved to form a second solution. The second acid solution may be hydrochloric acid, nitric acid or sulfuric acid, etc., and the second acid solution may be the same or different from the first acid solution, but its volume may be much less. In this embodiment, the second acid solution is dilute hydrochloric acid having a concentration of 18% by weight (wt%), a volume of 50 cc, and a temperature of 25 ° C, which can dissolve the metal iron to Forming a second solution. Step S107: filtering and drying the second solution to obtain a second powder. The filtering step is the same as the filtering step of step S104, and filtering is performed by using a filter paper, wherein the filter paper has an aperture. (Pore) is 2~7 μιη, Preferably, the filter paper used in this step can be the same as step sl4, but it can be understood that the filter paper of this step can be different from step S104. In this embodiment, the second is cooled first. After the solution, the second solution is filtered by using a filter paper having a pore diameter of 4 to 5 μm, and the residue on the filter paper is placed in the high temperature furnace to be dried to completely ash about 8 ° C to obtain a first a second powder comprising the alumina intervening material, wherein the alumina intercalation particle size is greater than 0.5 μm. Then, if necessary, the composition of the oxide can be quantitatively analyzed by an instrument and The advantage of the present invention is that the time taken for the entire separated steel to be mediated is reduced by 116092.doc -10- 200827457 short 'the ratio of the present method can be saved by half compared with the conventional method, and the method of the present invention is utilized. Separation, s. The particle size of this object can be as small as 〇·5 μηι, so it can be used as a barrier. Applied to small sizes smaller than ~
C 惟上述實施例僅為說明本發明之原理及其功效，而非用 以限制本發明。iUb，習於此技術之人士對上述實施例進 行修改及變化仍不脫本發明之精神。本發明之權利範圍應 如後述之申請專利範圍所列。 【圖式簡單說明】 圖1顯示本發明分離鋼中介在物的方法之較佳實施例之 流程圖。 116092.docThe above-described embodiments are merely illustrative of the principles of the invention and its effects, and are not intended to limit the invention. iUb, the person skilled in the art can modify and change the above embodiments without departing from the spirit of the invention. The scope of the invention should be as set forth in the appended claims. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing a preferred embodiment of the method for separating steel intermediaries of the present invention. 116092.doc