TW201807408A - Method for measuring solidification temperature of slag during temperature rising process obtaining the solidification temperature of the slag by shaping the slag and observing change of shape during the temperature rising process - Google Patents

Method for measuring solidification temperature of slag during temperature rising process obtaining the solidification temperature of the slag by shaping the slag and observing change of shape during the temperature rising process Download PDF

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TW201807408A
TW201807408A TW105126695A TW105126695A TW201807408A TW 201807408 A TW201807408 A TW 201807408A TW 105126695 A TW105126695 A TW 105126695A TW 105126695 A TW105126695 A TW 105126695A TW 201807408 A TW201807408 A TW 201807408A
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slag
temperature
sample
powder
measuring
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TW105126695A
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TWI591328B (en
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蕭嘉賢
劉世賢
黃聰彥
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中國鋼鐵股份有限公司
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Abstract

A method for measuring solidification temperature of slag during temperature rising process includes the following steps: heating and melting slag powders and oxide composition powders of magnesium oxide, aluminum oxide, calcium oxide, silicon dioxide and titanium dioxide after mixing; cooling the melting product to form slag block; grinding the slag block into powder to obtain a powder sample; mixing the powder sample, water and adhesive to form a cylinder sample; heating the cylinder sample to observe change of shape of the cylinder sample during the heating process; and setting a temperature of the cylinder sample starting to deform as a solidification temperature of the slag. The method obtains the solidification temperature of the slag by shaping the slag and observing change of shape during the temperature rising process. The obtained solidification temperature can precisely represent fluidity of the slag.

Description

一種測定爐渣升溫過程中固化溫度的方法Method for measuring curing temperature during slag heating

本發明是有關於一種爐渣流動性的量測方法,特別是指一種以觀察法直接觀察爐渣在升溫過程中的形態變化得到爐渣的固化溫度,繼而準確地得知爐渣流動性的量測方法。The present invention relates to a measurement method for slag fluidity, and particularly to a measurement method for directly observing the morphological change of slag during the heating process by an observation method to obtain the solidification temperature of the slag, and then accurately know the slag fluidity.

爐渣是各種火法冶金工藝中礦石及原燃料中的雜質成分經過冶煉及高溫後與金屬分離得到的產物。爐渣在高溫下的流動性是非常重要的性質,爐渣具有良好的流動性就能夠與金屬順利的分離,同時為去除金屬中雜質的反應提供良好的動力學條件。因此如何準確地控制爐渣的流動性,是冶金領域中極為重要的課題。Slag is a product obtained by smelting and separating high temperature impurities from metals in various pyrometallurgical processes. The slag fluidity at high temperature is a very important property. The slag has good fluidity and can be smoothly separated from the metal, and at the same time, it provides good kinetic conditions for the reaction of removing impurities in the metal. Therefore, how to accurately control the fluidity of slag is an extremely important subject in the field of metallurgy.

現有控制爐渣流動性的方法是以量測爐渣的熔化溫度來進行,該熔化溫度是以降溫方式進行,並以黏度分析法得到。熔化溫度為黏度突然急遽上升的溫度點,就降溫過程的材料結構而言,應是接近完全固化,黏度計的轉子扭力方會突然增大。熔化性溫度在冶金科學中尚未標準規範定義,沒有給定量測黏度和溫度的範圍,目前主要利用定斜率法、定黏度法及兩切線相交法三種方式來定義。但是,上述三種方法皆無法準確定義熔化溫度,導致依所定義熔化溫度進行爐渣流動性控制時產生無法準確控制流動性的問題。The existing method for controlling the fluidity of the slag is to measure the melting temperature of the slag, and the melting temperature is performed in a cooling manner and obtained by a viscosity analysis method. The melting temperature is the temperature at which the viscosity suddenly rises sharply. As far as the material structure of the cooling process is concerned, it should be almost completely solidified, and the rotor torque of the viscometer will suddenly increase. Melting temperature has not been defined by standard specifications in metallurgical science. There is no given range for measuring viscosity and temperature. Currently, three methods are used to define the fixed slope method, the fixed viscosity method and the intersection of two tangents. However, none of the above three methods can accurately define the melting temperature, resulting in a problem that the fluidity cannot be accurately controlled when the slag fluidity control is performed according to the defined melting temperature.

由以上說明可知,透過量測熔化溫度無法準確控制爐渣的流動性,因此仍有需要開發出一種能夠更簡便又準確地控制爐渣流動性的方法。As can be seen from the above description, the measurement of the melting temperature cannot accurately control the slag fluidity, so there is still a need to develop a method that can more simply and accurately control the slag fluidity.

因此,本發明之目的,即在提供一種測定爐渣升溫過程中固化溫度的方法,包含以下步驟:Therefore, an object of the present invention is to provide a method for determining a curing temperature during a slag heating process, which includes the following steps:

於是,本發明測定爐渣升溫過程中固化溫度的方法,包含以下步驟: 將爐渣粉末及一含有氧化鎂、氧化鋁、氧化鈣、二氧化矽及二氧化鈦的氧化物組成物粉末混合後加熱熔融,再使熔融得到的產物冷卻成型為一爐渣塊,再將該爐渣塊研磨成粉以製得一粉末樣品; 將該粉末樣品、水及黏結劑混合後造塊成型,得到一柱體樣品;及 加熱該柱體樣品,同時觀察在加熱過程中該柱體樣品的形狀變化,將該柱體樣品的形狀開始變化時的變形溫度做為爐渣的固化溫度。Therefore, the method for measuring the curing temperature in the slag heating process according to the present invention includes the following steps: slag powder and an oxide composition powder containing magnesium oxide, aluminum oxide, calcium oxide, silicon dioxide, and titanium dioxide are mixed and heated to melt, and then The molten product is cooled and formed into a slag block, and the slag block is ground into powder to obtain a powder sample; the powder sample, water and a binder are mixed to form a block to obtain a column sample; and heating For the pillar sample, the shape change of the pillar sample during the heating process was observed, and the deformation temperature when the shape of the pillar sample started to change was taken as the solidification temperature of the slag.

本發明之功效在於:該測定爐渣升溫過程中固化溫度的方法透過將爐渣造塊成型並直接觀察其受熱於升溫過程中的形態變化得到爐渣的固化溫度,所得到的固化溫度能夠較準確地呈現爐渣的流動性,更利於控制爐渣的流動性。The effect of the present invention is that the method for measuring the curing temperature during the slag heating process obtains the slag curing temperature by forming the slag into a block and directly observing its morphological change during heating. The obtained curing temperature can be presented more accurately. The slag fluidity is more conducive to controlling the slag fluidity.

以下將就本發明內容進行詳細說明:The following will describe the content of the present invention in detail:

較佳地,將在加熱過程中該柱體樣品的形狀變為半圓體時的溫度做為爐渣的液化溫度。Preferably, the temperature at which the shape of the column sample changes to a semi-circular body during heating is taken as the liquefaction temperature of the slag.

較佳地,將在加熱過程中該柱體樣品開始流動時的溫度做為爐渣的流動溫度。Preferably, the temperature at which the column sample starts to flow during the heating process is taken as the flow temperature of the slag.

較佳地,該加熱的方式是以10℃/min的速度升溫至1500℃。Preferably, the heating is performed at a rate of 10 ° C / min to 1500 ° C.

較佳地,該粉末樣品的平均粒徑範圍為50μm至100μm 。Preferably, the average particle size of the powder sample ranges from 50 μm to 100 μm.

較佳地,該爐渣粉末的平均粒徑範圍為50μm至100μm 。Preferably, the average particle size of the slag powder ranges from 50 μm to 100 μm.

較佳地,該氧化物組成物粉末的平均粒徑範圍為50μm至75μm 。Preferably, the average particle diameter of the oxide composition powder ranges from 50 μm to 75 μm.

較佳地,該爐渣是高爐的最終渣。該高爐的最終渣含有CaO、SiO2 、Al2 O3 、MgO、TiO2Preferably, the slag is the final slag of the blast furnace. The final slag of the blast furnace contains CaO, SiO 2 , Al 2 O 3 , MgO, and TiO 2 .

透過添加該氧化物組成物配置出所需之化學組成的爐渣。較佳地,該氧化物組成物含有氧化鎂、氧化鋁、氧化鈣、二氧化矽及二氧化鈦。以該氧化物組成物的總量為100 wt%,該氧化鎂的含量範圍為3至11wt%。以該氧化物組成物的總量為100 wt%,該氧化鋁的含量範圍為10至18wt%。以該氧化物組成物的總量為100 wt%,該氧化鈣的含量範圍為39至46 wt%。以該氧化物的總量為100 wt%,該二氧化矽的含量範圍為32至41 wt%。以該氧化物的總量為100 wt%,該二氧化鈦的含量範圍為0.3至4.5 wt%。By adding the oxide composition, a slag having a desired chemical composition is configured. Preferably, the oxide composition contains magnesium oxide, aluminum oxide, calcium oxide, silicon dioxide, and titanium dioxide. The total content of the oxide composition is 100 wt%, and the content of the magnesium oxide ranges from 3 to 11 wt%. The total content of the oxide composition is 100 wt%, and the content of the alumina ranges from 10 to 18 wt%. The total content of the oxide composition is 100 wt%, and the content of the calcium oxide ranges from 39 to 46 wt%. The total content of the oxide is 100 wt%, and the content of the silicon dioxide ranges from 32 to 41 wt%. The total content of the oxide is 100 wt%, and the content of the titanium dioxide ranges from 0.3 to 4.5 wt%.

較佳地,該柱體樣品是一直徑3.5釐米及高度3.5釐米的圓柱體樣品。Preferably, the cylindrical sample is a cylindrical sample with a diameter of 3.5 cm and a height of 3.5 cm.

較佳地,該黏結劑是澱粉。較佳地,以該粉末樣品、水及澱粉的總量為100wt%,該粉末樣品的用量範圍為70至77 wt%,該水的用量範圍為20至25 wt%,該澱粉的用量範圍為3至5 wt%。Preferably, the binding agent is starch. Preferably, the total amount of the powder sample, water and starch is 100 wt%, the amount of the powder sample is in the range of 70 to 77 wt%, the amount of water is in the range of 20 to 25 wt%, and the amount of the starch is 3 to 5 wt%.

本發明將就以下實施例來作進一步說明,但應瞭解的是,該實施例僅為例示說明之用,而不應被解釋為本發明實施之限制。The present invention will be further described with reference to the following examples, but it should be understood that this example is for illustrative purposes only and should not be construed as a limitation on the implementation of the present invention.

[實施例1][Example 1]

將煉鋼現場取得的高爐最終渣(final slag)先磨成平均粒徑範圍為50μm至100μm 的細粉,再與平均粒徑範圍為50μm至75μm的氧化物組成物粉末(含有39至46wt%的CaO、3至11 wt%的MgO、10至18 wt%的Al2 O3 、32至41wt%的SiO2 及0.3至4.5wt%的TiO2 )混合後放入一高溫爐內以1550℃加熱熔融,將熔融後的產物從該高溫爐中取出以冷卻成塊,得到一爐渣塊。將該爐渣塊敲碎並研磨成粉,得到一平均粒徑範圍為75μm的粉末樣品,並以感應耦合電漿原子發射光譜分析儀(ICP-AES)的方式對該待測粉末樣品進行成份分析。將該粉末樣品、水及澱粉(粉末樣品70至77 wt%,水:20至25 wt%,澱粉:3至5 wt%)混合後加壓成塊,製成一圓柱體樣品(直徑3.5釐米,高度3.5釐米)。將該圓柱體樣品置於一高溫爐(德國dataphysis公司,型號:OCA 15LHT plus)的爐管內加熱,加熱方式為10℃/min的速度升溫至1500℃,並在加熱升溫過程中使用一高溫光學影像拍攝器(德國dataphysis公司,型號:OCA 15LHT plus)拍攝該圓柱體樣品隨著溫度上升而產生的形狀變化。其中,圖1A是還未開始加熱時該圓柱體的照片;圖2A是在加熱過程中該圓柱體樣品的形狀剛開始變化時的照片,此時的溫度稱為變形溫度(deformation temperature);圖3A是在加熱過程中該圓柱體樣品的形狀變為半圓體時的照片,此時的溫度稱為液化溫度(liquidus temperature);圖4A是在加熱過程中該圓柱體樣品開始流動時的照片,此時的溫度稱為流動溫度(flow temperature)The final slag of the blast furnace obtained at the steelmaking site is first ground into a fine powder with an average particle size ranging from 50 μm to 100 μm, and then with an oxide composition powder with an average particle size ranging from 50 μm to 75 μm (containing 39 to 46 wt% of CaO, 3 to 11 wt% of MgO, 10 to 18 wt% of Al 2 O 3, 32 to 41wt% of SiO 2 and 0.3 to 4.5wt% of TiO 2) are mixed into a high-temperature furnace at 1550 deg.] C The mixture is heated and melted, and the molten product is taken out of the high-temperature furnace to be cooled into a block to obtain a slag block. The slag block was crushed and ground into powder to obtain a powder sample with an average particle size range of 75 μm, and the component analysis of the powder sample to be tested was performed by an inductively coupled plasma atomic emission spectrometer (ICP-AES). . The powder sample, water and starch (powder sample 70 to 77 wt%, water: 20 to 25 wt%, starch: 3 to 5 wt%) were mixed and pressed into a block to form a cylindrical sample (3.5 cm in diameter). , Height 3.5 cm). The cylindrical sample was heated in a furnace tube of a high temperature furnace (German dataphysis company, model: OCA 15LHT plus). The heating method was heated to 1500 ° C at a rate of 10 ° C / min, and a high temperature was used during the heating and heating process. An optical image capture device (dataphysis, Germany, model: OCA 15LHT plus) captures the shape change of the cylindrical sample as the temperature rises. Among them, FIG. 1A is a photograph of the cylinder before the heating has started; FIG. 2A is a photograph of the shape of the cylinder sample when the heating process has just started to change, and the temperature at this time is called the deformation temperature; 3A is a photograph when the shape of the cylindrical sample becomes a semicircular body during the heating process, and the temperature at this time is called a liquidus temperature (liquidus temperature); FIG. 4A is a photograph when the cylindrical sample starts to flow during the heating process, The temperature at this time is called the flow temperature

[實施例2至31][Examples 2 to 31]

以與實施例1相同的步驟流程進行實施例2至31,差別在於使用不同的氧化物組成物粉末。Examples 2 to 31 were performed in the same step flow as Example 1, except that different oxide composition powders were used.

實施例1至31的變形溫度的量測結果如表1至表5中所示。The measurement results of the deformation temperatures of Examples 1 to 31 are shown in Tables 1 to 5.

[利用已知黏度分析法量測熔化溫度][Measure the melting temperature with a known viscosity analysis method]

將實施例1至31的粉末樣品進行黏度分析法,得到一黏度隨溫度變化的曲線,取該曲線的兩端的切線,並將兩條切線的相交點做為熔化溫度(為爐渣熔化後能自由流動的溫度,黏度突然急遽上升的溫度點),將得到的熔化性溫度與實施例1至31得到的變形溫度做比較。其中,黏度分析法的步驟如下所述:將110克的粉末樣品倒入一石墨坩堝內,再將該石墨坩堝放在一高溫爐渣黏度量測儀(廠商:BROOKFIELD,型號:MODEL DV-II)的樣品支架上,以升降裝置將坩堝上升至直立式高溫爐內進行加熱,直到坩堝內的粉末樣品完全熔融後,再以升降裝置將扭力式黏度計下降至定位,進行隨溫度下降的黏度量測,並同時獲得扭力隨時間上升以及溫度隨時間下降的數據,對照扭力與黏度的校正曲線得到該黏度隨溫度變化的曲線。測得的實施例1至31的熔化溫度如表1至表5中所示。The powder samples of Examples 1 to 31 were subjected to a viscosity analysis method to obtain a curve of viscosity as a function of temperature. The tangent lines at both ends of the curve were taken, and the intersection of the two tangent lines was used as the melting temperature. The flow temperature, the temperature at which the viscosity suddenly rises sharply), and the obtained melting temperature is compared with the deformation temperature obtained in Examples 1 to 31. The steps of the viscosity analysis method are as follows: pour 110 grams of powder sample into a graphite crucible, and then place the graphite crucible in a high temperature slag viscosity measuring instrument (manufacturer: BROOKFIELD, model: MODEL DV-II) On the sample holder, the crucible is lifted into an upright high-temperature furnace by a lifting device to be heated until the powder sample in the crucible is completely melted, and then the torque viscometer is lowered to the position by the lifting device, and the viscosity measurement with temperature is performed. Measurement, and at the same time to obtain the data of the torque increase with time and the temperature decrease with time, the curve of the change of viscosity with temperature is obtained by comparing the correction curve of torque and viscosity. The measured melting temperatures of Examples 1 to 31 are shown in Tables 1 to 5.

表1 Table 1

表2 Table 2

表3 table 3

表4 Table 4

表5 table 5

從表1至表5可知,實施例1至31的變形溫度與熔化溫度的差值在0至36℃間,因此可將變形溫度視為爐渣的固化溫度。As can be seen from Tables 1 to 5, the difference between the deformation temperature and the melting temperature of Examples 1 to 31 is between 0 and 36 ° C. Therefore, the deformation temperature can be regarded as the solidification temperature of the slag.

綜上所述,本發明爐渣流動性的量測方法透過將爐渣造塊成型,直接觀察其受熱於升溫過程中的形態變化得到爐渣的固化溫度,所得到的固化溫度能夠較準確地呈現爐渣的流動性,故確實能達成本發明之目的。In summary, the method for measuring the slag fluidity of the present invention obtains the slag solidification temperature by forming the slag into pieces and directly observing the morphological changes during heating. The solidification temperature obtained can accurately represent the slag's temperature. Liquidity, so it can indeed achieve the purpose of the invention.

惟以上所述者,僅為本發明之實施例而已,當不能以此限定本發明實施之範圍,凡是依本發明申請專利範圍及專利說明書內容所作之簡單的等效變化與修飾,皆仍屬本發明專利涵蓋之範圍內。However, the above are only examples of the present invention. When the scope of implementation of the present invention cannot be limited in this way, any simple equivalent changes and modifications made in accordance with the scope of the patent application and the content of the patent specification of the present invention are still Within the scope of the invention patent.

本發明之其他的特徵及功效,將於參照圖式的實施方式中清楚地呈現,其中: [圖1A]是本發明爐渣流動性的量測方法的實施例1的圓柱體樣品的照片; [圖1B]是圖1A照片對應的方格圖; [圖2A]是該實施例1的圓柱體樣品在加熱過程中形狀剛開始變化時的照片; [圖2B]是圖2A照片對應的方格圖; [圖3A]是該實施例1的圓柱體樣品在加熱過程中形狀變為半圓體時的照片 [圖3B]是圖3A照片對應的方格圖; [圖4A]是該實施例1的圓柱體樣品在加熱過程中開始流動時的照片;及 [圖4B]是圖4A照片對應的方格圖。Other features and effects of the present invention will be clearly presented in the embodiment with reference to the drawings, in which: [Fig. 1A] is a photograph of a cylindrical sample of Embodiment 1 of the method for measuring slag fluidity of the present invention; Fig. 1B] is a grid diagram corresponding to the photograph of Fig. 1A; [Fig. 2A] is a photograph of the cylindrical sample of the first embodiment when the shape of the sample has just started to change; [Fig. 2B] is a grid corresponding to the photograph of Fig. 2A [Fig. 3A] is a photograph of the cylindrical sample of Example 1 when the shape becomes a semi-circular body during heating [Fig. 3B] is a grid diagram corresponding to the photograph of Fig. 3A; [Fig. 4A] is Example 1 A photo of the cylindrical sample at the beginning of the flow during heating; and [Fig. 4B] is a graph corresponding to the photo of Fig. 4A.

Claims (7)

一種測定爐渣升溫過程中固化溫度的方法,包含以下步驟: 將爐渣粉末及一含有氧化鎂、氧化鋁、氧化鈣、二氧化矽及二氧化鈦的氧化物組成物粉末混合後加熱熔融,再使加熱熔融得到的產物冷卻成型為一爐渣塊,再將該爐渣塊研磨成粉以製得一粉末樣品; 將該粉末樣品、水及黏結劑混合後造塊成型,得到一柱體樣品;及 加熱該柱體樣品,同時觀察在加熱過程中該柱體樣品的形狀變化,將該柱體樣品的形狀開始變化時的變形溫度做為爐渣的固化溫度。A method for measuring the curing temperature during the slag heating process includes the following steps: mixing and heating and melting the slag powder and an oxide composition powder containing magnesium oxide, aluminum oxide, calcium oxide, silicon dioxide, and titanium dioxide, and then heating and melting The obtained product is cooled and formed into a slag block, and the slag block is ground into powder to obtain a powder sample; the powder sample, water and a binder are mixed to form a block to obtain a column sample; and the column is heated; At the same time, observe the shape change of the pillar sample during the heating process, and the deformation temperature when the shape of the pillar sample starts to change is used as the solidification temperature of the slag. 如請求項1所述的測定爐渣升溫過程中固化溫度的方法,其中,該加熱的方式是以10℃/min的速度升溫至1500℃。The method for measuring a curing temperature in a slag heating process according to claim 1, wherein the heating method is to raise the temperature to 1500 ° C at a rate of 10 ° C / min. 如請求項1所述的測定爐渣升溫過程中固化溫度的方法,其中,該粉末樣品的平均粒徑範圍為50 μm至100 μm。The method for measuring a curing temperature in a slag heating process according to claim 1, wherein the average particle size of the powder sample ranges from 50 μm to 100 μm. 如請求項1所述的測定爐渣升溫過程中固化溫度的方法,其中,該爐渣粉末的平均粒徑範圍為50 μm至100 μm。The method for measuring a curing temperature in a slag heating process according to claim 1, wherein the average particle diameter of the slag powder ranges from 50 μm to 100 μm. 如請求項1所述的測定爐渣升溫過程中固化溫度的方法,其中,該氧化物組成物粉末的平均粒徑範圍為50 μm至75 μm。The method for measuring a curing temperature in a slag heating process according to claim 1, wherein the average particle diameter of the oxide composition powder ranges from 50 μm to 75 μm. 如請求項1所述的測定爐渣升溫過程中固化溫度的方法,其中,該爐渣是高爐的最終渣。The method for measuring a curing temperature in a slag heating process according to claim 1, wherein the slag is a final slag of a blast furnace. 如請求項1所述的測定爐渣升溫過程中固化溫度的方法,其中,該柱體樣品是一直徑3.5釐米及高度3.5釐米的圓柱體樣品。The method for measuring a curing temperature in a slag heating process according to claim 1, wherein the cylindrical sample is a cylindrical sample having a diameter of 3.5 cm and a height of 3.5 cm.
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Publication number Priority date Publication date Assignee Title
CN111957917A (en) * 2020-09-17 2020-11-20 贵州理工学院 Device and method for obtaining continuous casting mold flux solidified slag film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111957917A (en) * 2020-09-17 2020-11-20 贵州理工学院 Device and method for obtaining continuous casting mold flux solidified slag film

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