CN109520777B - Silicon carbide sampling spoon and manufacturing process - Google Patents
Silicon carbide sampling spoon and manufacturing process Download PDFInfo
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- CN109520777B CN109520777B CN201910018549.6A CN201910018549A CN109520777B CN 109520777 B CN109520777 B CN 109520777B CN 201910018549 A CN201910018549 A CN 201910018549A CN 109520777 B CN109520777 B CN 109520777B
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Abstract
The invention discloses a silicon carbide sampling spoon, which has the following indexes: high temperature resistant 1300 ℃ 1380 ℃; the porosity is less than 0.1%; the density is 2.95-3.10 g/cm3. Simultaneously discloses a manufacturing process of the silicon carbide sampling spoon, which comprises the steps of early-stage mould making and slip casting, middle-stage machining and post-processing, wherein the slurry used in the steps of early-stage mould making and slip casting comprises the following components in parts by weight: 75-85 parts of silicon carbide micro powder, 58-62 parts of softened water, 3.6-4.4 parts of carbon black, 2.7-3.3 parts of carbon fiber, 2.7-3.3 parts of silicon nitride micro powder, 2.7-3.3 parts of metal tungsten micro powder, 2.7-3.3 parts of manganese dioxide powder, 2.7-3.3 parts of titanium oxide powder, 3.6-4.4 parts of dispersing agent and 6.5-7.5 parts of binding agent.
Description
Technical Field
The invention relates to a sampling spoon for containing molten metal after metal melting, in particular to a silicon carbide sampling spoon in a metal melting and casting process (such as aluminum melting) and a novel manufacturing process, and belongs to the technical field of metal casting.
Background
The molten metal sampling spoon is specially used for taking out liquid metal in a furnace or a ladle so as to be convenient for assay and analysis. The sampling spoon mainly comprises a spoon body and a spoon handle, and the spoon handle is connected with the spoon body in a seamless mode. The spoon body is a cavity with an opening at one end, and the other side surface of the cavity corresponding to the opening is connected with the spoon handle. The steel pipe is required to be welded tightly with the spoon body in an oblique angle, and the steel pipe cannot be broken flat and welded with the spoon body so as to increase the use strength.
For the sampling spoon, a molten metal sample has the characteristics of high temperature, corrosivity, oxidability and the like, so when the sampling spoon is selected, the material for manufacturing the sampling spoon not only needs to have excellent high-temperature resistance, but also needs to have the performances of corrosion resistance and oxidation resistance at high temperature, and has a long service life, and the sampling spoon can be easily manufactured into various sizes and shapes according to actual requirements. At present, 316 stainless steel, 304 stainless steel, stainless steel lining refractory materials, graphite and the like exist in the sampling spoon.
The following should be noted for the selection of the sampling spoon:
l, whether the material of the sampling spoon is suitable for the high-temperature, corrosive and oxidative environment of the required melt or not;
2. the size and shape of the opening are easy to take liquid from the metal melting vessel and pour;
3. the sampling spoon should have smooth inner and outer walls to prevent the molten liquid from sticking on the sampling spoon;
4. during sampling, a sampling scoop port is perpendicular to the molten liquid, and the full-width full-thickness ore pulp flow is transversely intercepted at a constant speed;
5. a certain and equal time interval is needed during sampling;
6. the sampling spoon needs to be checked regularly to prevent the sample liquid from being polluted by slag falling caused by oxidation or damage of the material of the sampling spoon due to high temperature or corrosion of the molten liquid;
7. a special sampling spoon is configured at each sampling point;
8. the volume of the sampling spoon should be larger than the volume required for the melt to be intercepted once.
Due to the functional requirements of the sampling spoon, the material and the use environment of the prior sampling spoon are complex, the appearance structure is various, the precision requirement is higher, the surface smoothness requirement is strict, and the wall thickness of the whole product component is not uniform. Like a stainless steel sampling spoon, is easy to be oxidized and corroded by molten metal, and has short service life and high replacement frequency; the stainless steel lining refractory material sampling spoon is easy to be baked by high-temperature molten metal, the lining material is easy to peel off, the sampling accuracy is poor, the service life is influenced, and slag is easy to fall to pollute the molten metal.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a silicon carbide sampling spoon used in a metal smelting process, so as to overcome the technical defects that the existing material is easy to corrode and oxidize, high in porosity, poor in accuracy, easy to drop slag to pollute a sample, incapable of realizing production of a special-shaped sampling spoon and the like.
In order to solve the problems, the invention adopts the following technical scheme: a silicon carbide sampling spoon having the following indices:
high temperature resistant 1300 ℃ 1380 ℃;
the porosity is less than 0.1%;
the density is 2.95-3.10 g/cm3。
The silicon carbide material is selected to manufacture the sampling spoon, so that the sampling spoon not only has excellent high-temperature resistance, but also can resist corrosion and oxidation, and can be widely applied to metal metallurgy even in high-temperature and high-corrosivity metal solutionIn the smelting industry, the silicon carbide sampling spoon is an important part required for realizing metal sampling and accurate measurement, and the density of the silicon carbide sampling spoon is 2.95g/cm in terms of weight3 - 3.2g /cm3The product with the same size is lighter than stainless steel by more than 2 times, so the use is more convenient; the service life is long, the porosity of the silicon carbide ceramic is less than 0.1%, and the porosity of the common refractory material is 18% -30%, so that the silicon carbide ceramic is more resistant to oxidation and corrosion.
The invention also provides a manufacturing process of the silicon carbide sampling spoon, which comprises the steps of early-stage mould making and slip casting, middle-stage machining and post-processing, wherein the slurry used in the steps of early-stage mould making and slip casting comprises the following components in parts by weight:
75-85 parts of silicon carbide micro powder, 58-62 parts of softened water, 3.6-4.4 parts of carbon black, 2.7-3.3 parts of carbon fiber, 2.7-3.3 parts of silicon nitride micro powder, 2.7-3.3 parts of metal tungsten micro powder, 2.7-3.3 parts of manganese dioxide powder, 2.7-3.3 parts of titanium oxide powder, 3.6-4.4 parts of dispersing agent and 6.5-7.5 parts of binding agent.
The following is a further optimization of the present invention to the above scheme: the intermediate machining step comprises the following steps: drying a blank body of the spoon body, and then performing surface finishing; and secondly, processing the spoon handle by using a machine tool.
Further optimization: and step two, processing the shape of the spoon handle to a tolerance range of +/-1 mm by adopting a machine tool.
Further optimization: and secondly, processing the appearance of the spoon handle by adopting a machine tool until the surface roughness is Ra1.6-3.2.
Further optimization: the post-processing step comprises the steps of: a. drying the formed green body in a high-temperature drying chamber, and then loading into a furnace for sintering; b. and (5) sand blasting treatment.
Further optimization: in the step a, the temperature in the high-temperature drying chamber is 82-97 ℃.
Further optimization: in the step a, the drying time of the formed blank body in a high-temperature drying chamber is 8-10 hours.
Further optimization: in the step a, the formed blank is dried in a high-temperature drying chamber until the moisture content is lower than 2 percent and then sintered.
Further optimization: the sand blasting treatment makes the surface roughness of the product Ra0.2-1.6.
The invention can accurately finish the manufacture of the inner and outer structural forms of the sampling spoon, and can produce the sampling spoon which is special, asymmetric and uneven; and the product process is simple and the yield is high.
The following is a comparison of the present invention with the prior art:
the invention is further illustrated with reference to the following figures and examples.
Drawings
FIG. 1 is a schematic diagram of a sampling spoon according to an embodiment of the present invention;
FIG. 2 is a top view of FIG. 1;
FIG. 3 is a schematic diagram of a sampling spoon according to an embodiment of the present invention;
FIG. 4 is a top view of FIG. 3;
FIG. 5 is a schematic diagram of a sampling spoon according to an embodiment of the present invention;
fig. 6 is a top view of fig. 5.
Detailed Description
Example 1 as shown in fig. 1 to 6, the silicon carbide sampling spoon includes a metal solution sampling spoon made of silicon carbide, so that the sampling spoon is corrosion-resistant, oxidation-resistant, low in porosity, high in accuracy and not easy to contaminate samples.
The silicon carbide sampling spoon is made of silicon carbide materials, has excellent high-temperature resistance, corrosion resistance and oxidation resistance, can be widely applied to the metal smelting industry even in high-temperature and high-corrosion metal solution, is an important part required for realizing metal sampling and accurate measurement, and has the density of 2.95g/cm in terms of weight3 -3.1g/cm3The product with the same size is lighter than stainless steel by more than 2 times, so the use is more convenient; long service life, the porosity of the silicon carbide ceramic is less than 0.1 percent, the porosity of the common refractory material is 18 to 30 percent, and the common refractory material is more oxidation-resistantAnd (4) corrosion resistance.
The invention also provides a manufacturing process of the silicon carbide sampling spoon, which comprises the following steps:
(1) manufacturing an inner bottom die and an outer bottom die: the manufacturing method of the inner bottom die and the outer bottom die of the spoon body and the spoon handle is completed by adopting a machining and manual process bonding method according to the structural sizes of the inner bottom die and the outer bottom die which are designed according to the structures of the spoon body and the spoon handle of the sampling spoon, wherein the outer bottom die is made of one of aluminum alloy, gypsum and epoxy resin, and the inner bottom die is made of one of aluminum alloy and gypsum.
(2) Production of the outer mold with the outsole mold: the outer mold is produced by using a plaster mold, an appropriate amount of soft soap water is uniformly wiped on an outer bottom mold, the outer bottom mold is placed in a mold with the shape of the plaster mold and fixed, gypsum slurry is prepared according to the proportion of 3:2 of gypsum powder and water, the gypsum and the water are fully mixed and then are stirred in vacuum for 1-3 minutes, impurities are screened out after the even stirring, the gypsum slurry is injected into the mold, slight oscillation is carried out to remove air bubbles, the gypsum slurry flows into each fine corner, the mold cavity is fully filled with the gypsum slurry at one time, after the gypsum slurry is solidified, the outer bottom mold is removed, the outer production mold is taken out, the outer gypsum production mold is dried in a drying chamber with the temperature of 40-50 ℃ for 3-4 days after being prepared, an electronic scale is used for weighing, the outer mold is taken out of the drying chamber when the water content of the mold is lower than 10%, the size of the mold is further measured by using the tool, and the tolerance of the mold is smaller than 1mm, the product can be used.
(3) Manufacturing a mold core: manufacturing a production inner mold by using the inner bottom mold, and manufacturing a mold core by using the production inner mold;
respectively molding inner bottom molds of the spoon body and the spoon handle to manufacture a spoon body and a spoon handle production inner mold, and respectively manufacturing mold cores of the spoon body and the spoon handle by using the inner bottom molds of the spoon body and the spoon handle; and manufacturing a mold core matched with the inner structures of the spoon body and the spoon handle according to the inner structures of the spoon body and the spoon handle.
(4) Slurry mixing and grouting forming: before starting up, checking whether a clutch, a brake and the like of the mixer for batching are good, cleaning the mixer barrel to a certain extent without foreign matters, and checking that the insulation and grounding of electrical equipment are kept intact;
when the machine is started for use, the stirrer is started to run in a no-load test mode, and after the machine runs normally, raw materials are added to stir to prepare the slurry, wherein the slurry comprises the following components in parts by weight: 60 parts of softened water, 80 parts of silicon carbide micro powder, 4 parts of carbon black, 3 parts of carbon fiber, 3 parts of silicon nitride micro powder, 3 parts of metal tungsten micro powder, 3 parts of manganese dioxide powder, 3 parts of titanium oxide powder, 4 parts of dispersing agent and 7 parts of binder;
wherein: most of the softened water in the raw materials volatilizes when demoulding and drying are carried out, the dispersing agent and the binder volatilize completely when the temperature is about 1000 +/-10 ℃, and the metallic silicon permeates into the blank body in the high-temperature reaction to react and fill all pores.
The raw materials are added into a stirrer and need to be stirred at a high speed under the working condition that the rotating speed is 850-900r/min, the stirring time needs more than 32 hours, all the raw materials are fully mixed to prepare slurry, and after the slurry is prepared, the slurry is taken out and filtered for later use;
placing the dried mould into a grouting area, adopting a solid grouting method to inject filtered slurry into the mould, determining the position, the number and the size of grouting holes on a production mould according to the structures of a spoon body and a spoon handle during grouting operation, fixing a mould core in a production external mould, and closing the mould and grouting after the central lines of the mould core and the spoon handle are necessarily kept coincident; the grouting speed is reasonably controlled in the grouting process, the grouting speed is about 25-40s/L, the phenomena of air bubbles, splash and the like are avoided when grout is injected, and the production mold is not vibrated to enable the grout to flow uniformly.
(5) And (3) drying: standing the grouted mould for 40-50 hours, opening the mould, taking out the silicon carbide blank, demoulding to obtain a formed blank of the spoon body and the spoon handle, naturally drying the blank outdoors for 5-8 hours if the outdoor temperature is above 15 ℃ and the air humidity is less than 70% RH, separating the mold core from the blank (blank) after drying, weighing the blank by using an electronic scale to calculate the predicted moisture content, then sending the blank into an electric heating drying chamber for drying at low temperature, setting the temperature of the electric heating drying chamber to be 25-29 ℃, drying for 40-60 hours, weighing the blank by using the electronic scale, calculating the moisture content, and taking out the blank when the moisture content is less than 5%.
(6) Machining and trimming biscuit
The method mainly comprises the following two steps:
step one, after a blank body of the spoon body is dried, trimming defects on the surface of the blank body manually;
secondly, setting the travel of a turning tool of a vertical or horizontal machine tool according to the size parameters of the spoon handle to be processed, such as length, diameter and the like, clamping the dried blank on a chuck of the machine tool, correcting the blank by a measuring tool, then a cutter is arranged on a cutter rest and is adjusted, then according to the size requirement of the spoon handle appearance, after the angle between the turning tool and the blank axis is further corrected by a caliper and an angle ruler (measuring tool), a machine tool is started, the spoon handle appearance is processed by the turning tool, the measuring tool is continuously used for measuring the length, the diameter and other dimensions of the spoon handle in the processing process, the shape tolerance range of the spoon handle blank is ensured to be within +/-1 mm, comparing the measured surface of the blank with a surface roughness comparison sample block (sample block for short) according to vision and touch, ensuring that the surface roughness is between Ra1.6 and 3.2, and visually checking that the surface of the blank has no dark lines, damages, air holes and the like;
after the whole biscuit is machined, the spoon handle and the spoon body are spliced, and then the formed dry biscuit with the defective surface is trimmed.
(7) And (3) sintering: sending the trimmed molded blank into a high-temperature drying chamber, drying at 82-97 ℃ for 8-10 hours, measuring the moisture content of the blank to be less than 2% through the weight change of the blank, then putting the blank into a vacuum sintering furnace, pouring metal silicon into gaps and the bottom of a product, wherein the weight of the metal silicon (the purity of the metal silicon is more than 99.5%) which is dispersedly placed is about 1 time of that of the blank of the product, and the weight difference is not more than 25% through up-and-down fluctuation.
Before a vacuum sintering furnace is started, firstly, connecting cooling water, wherein the water pressure of the cooling water is kept between 0.1 and 0.2 Mpa, the water outlet temperature is less than or equal to 45 ℃, adjusting the flow of each water valve on the vacuum sintering furnace to a proper position, then filling compressed air into the vacuum sintering furnace to ensure that the pressure in the vacuum sintering furnace reaches 0.3 to 0.5Mpa, then setting a heating process curve through a temperature controller (FP23) on the vacuum sintering furnace, and then vacuumizing the vacuum sintering furnace to ensure that the vacuum degree in the furnace is reduced to between 10 and 50 Pa;
then heating, operating an FP23 heating program, flushing industrial nitrogen (with the purity of more than 99.6%) into the vacuum sintering furnace after the heating is started, opening an exhaust fan and a micro-flushing valve on the vacuum sintering furnace when the vacuum sintering furnace is inflated to a set upper limit (1 +/-0.05 Kpa), adjusting the air inflow of a rotor flowmeter on the micro-flushing valve to be 400 +/-5L/h, giving an alarm when the temperature rises to 800 ℃, automatically closing the micro-flushing valve and the exhaust valve, releasing the alarm on an alarm interface, closing the exhaust fan on a monitoring interface, continuously raising the temperature to 1700 +/-5 ℃, vacuumizing to 50-200pa, and observing the temperature change condition displayed by an infrared thermometer in the hot zone at any time through an observation window on the furnace body by an operator;
when the temperature in the vacuum sintering furnace rises to 1410 ℃, the metallic silicon begins to melt, the metallic silicon continues to melt and generate steam along with the continuous rise of the temperature, the steam is adsorbed and permeated into a silicon carbide blank body, carbon in the blank body reacts with the permeated Si to generate beta-SiC, the beta-SiC is combined with alpha-SiC (silicon carbide micro powder), and free Si fills pores to form a high-compactness ceramic material;
when the temperature reaches 1700 +/-5 ℃, the operation of the heating program is finished, the heating system of the vacuum furnace (vacuum sintering furnace) is automatically closed and stopped, after the constant temperature is waited for 0.5-1.5 hours, nitrogen (with the purity of more than 99.6%) is filled to 1 +/-0.05 Kpa and cooled, when the temperature is lower than 600-700 ℃, the air cooling system on the vacuum sintering furnace can be opened to assist cooling, and after the tapping temperature (below about 150 ℃), the air cooling system is closed to prepare for tapping.
(8) Sand blasting treatment: cooling the sintered product discharged from the furnace to normal temperature (about 10-45 ℃), separating the sintered product from the silica sand, putting the product into a sand blasting machine, blowing the silica sand to move by using gas generated by a hollow press in the sand blasting machine, enabling the silica sand to be in contact friction with the surface of the product, removing the silicon metal adhered to the surface of the product, enabling the surface of the product to be smooth and clean, and comparing the surface roughness comparison sample block (sample block for short) with the measured surface of the product according to vision and touch to ensure that the surface roughness of the product is Ra0.2-1.6; namely, the surface of the product is free from adhering metal silicon and other visible foreign matters, and then the product is taken out, stored and packaged after being cleaned.
The steps (1) to (5) are the steps of early-stage molding and slip casting, the step (6) is the step of middle-stage machining, and the steps (7) and (8) are the steps of post-processing.
Example 2, in the step (4) of example 1, the slurry comprises the following components in parts by weight: 58 parts of softened water, 75 parts of silicon carbide micro powder, 3.6 parts of carbon black, 2.7 parts of carbon fiber, 2.7 parts of silicon nitride micro powder, 2.7 parts of metal tungsten micro powder, 2.7 parts of manganese dioxide powder, 2.7 parts of titanium oxide powder, 3.6 parts of dispersing agent and 6.5 parts of binder; and a silicon carbide sampling spoon was made using the process described in example 1.
Example 3, in the step (4) of example 1, the slurry comprises the following components in parts by weight: 62 parts of softened water, 85 parts of silicon carbide micro powder, 4.4 parts of carbon black, 3.3 parts of carbon fiber, 3.3 parts of silicon nitride micro powder, 3.3 parts of metal tungsten micro powder, 3.3 parts of manganese dioxide powder, 3.3 parts of titanium oxide powder, 4.4 parts of dispersing agent and 7.5 parts of binder; and a silicon carbide sampling spoon was made using the process described in example 1.
The invention can accurately finish the manufacture of the inner and outer structural forms of the sampling spoon, and can produce the sampling spoon which is special, asymmetric and uneven; and the product process is simple and the yield is high.
The following is a comparison of the present invention with the prior art:
| material of | 304/316 stainless steel | Silicon carbide |
| Density g/cm3 | 7.70-8.00 | 2.95-3.10 |
| Production method | Rolling of | Grouting |
| Product structure | Simple | Complexity of |
| Corrosion resistance | In general | Superior food |
| Resistance to oxidation | In general | Superior food |
| High temperature resistance | The use temperature of 304 stainless steel is below 800 ℃, and the use temperature of 316 stainless steel is below 1000 DEG C | The use temperature can reach 1380 DEG C |
| Service life | Less than 30 days | Over 60 days |
Having shown and described the basic principles and essential features of the invention and its advantages, it will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore intended that the embodiments be considered as illustrative and not restrictive in all respects, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (2)
1. The manufacturing process of the silicon carbide sampling spoon is characterized in that: the silicon carbide sampling spoon manufactured by the manufacturing process has the following indexes:
high temperature resistant 1300 ℃ 1380 ℃;
the porosity is less than 0.1%;
the density is 2.95-3.10 g/cm3；
The manufacturing process specifically comprises the steps of primary molding and slip casting, intermediate machining and post-processing;
the slurry used in the early molding and slip casting steps comprises the following components in parts by weight:
75-85 parts of silicon carbide micro powder, 58-62 parts of softened water, 3.6-4.4 parts of carbon black, 2.7-3.3 parts of carbon fiber, 2.7-3.3 parts of silicon nitride micro powder, 2.7-3.3 parts of metal tungsten micro powder, 2.7-3.3 parts of manganese dioxide powder, 2.7-3.3 parts of titanium oxide powder, 3.6-4.4 parts of dispersing agent and 6.5-7.5 parts of binding agent;
the intermediate machining step comprises the following steps: drying a blank body of the spoon body, and then performing surface finishing; firstly, standing a grouted mould for 40-50 hours during drying, then demoulding to obtain a formed blank of a spoon body and a spoon handle, naturally drying for 5-8 hours in an environment with the temperature of more than 15 ℃ and the air humidity of less than 70% RH, separating a mold core from the blank after drying, weighing by using an electronic scale to calculate the predicted moisture content, and then drying at a low temperature in a heating and drying chamber, wherein the temperature of the electric heating and drying chamber is set to be 25-29 ℃, drying for 40-60 hours, calculating the moisture content after drying is finished, and taking out the blank when the moisture content is less than 5%;
secondly, processing the spoon handle by a machine tool; firstly, processing the shape of the spoon handle to a tolerance range of +/-1 mm; the surface roughness is Ra1.6-3.2, and the blank surface is checked to have no dark lines, damages and air holes;
after the whole biscuit is machined, splicing the spoon handle and the spoon body, and finishing the molded dry biscuit with the defective surface;
the post-processing step comprises the steps of: a. drying the formed green body in a high-temperature drying chamber, and then loading into a furnace for sintering; the temperature in the high-temperature drying chamber is 82-97 ℃; drying the formed blank in a high-temperature drying chamber for 8-10 hours; drying the formed blank in a high-temperature drying chamber until the moisture content is lower than 2%, and then sintering;
b. and (5) sand blasting treatment.
2. A process for manufacturing a silicon carbide sampling spoon as claimed in claim 1, wherein: the sand blasting treatment makes the surface roughness of the product Ra0.2-1.6.
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