CN111238891A - Preparation method of internal defects of reaction sintered silicon carbide ceramic - Google Patents
Preparation method of internal defects of reaction sintered silicon carbide ceramic Download PDFInfo
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- CN111238891A CN111238891A CN202010047539.8A CN202010047539A CN111238891A CN 111238891 A CN111238891 A CN 111238891A CN 202010047539 A CN202010047539 A CN 202010047539A CN 111238891 A CN111238891 A CN 111238891A
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Abstract
The invention provides a preparation method of internal defects of reaction sintered silicon carbide ceramics, which comprises the following steps: preparing two silicon carbide biscuit with same shape and size and flat surface; coating an inert inorganic substance on the surface of one porous silicon carbide biscuit according to the position of the designed defect, so that the shape and the size of the forming area coated with the inert inorganic substance are kept consistent with the shape and the size of the designed defect; coating organic binder on the rest positions of the surface of the porous silicon carbide biscuit with the prefabricated defects, flattening the surface of the porous silicon carbide biscuit again, butting and jointing the porous silicon carbide biscuit with another porous silicon carbide biscuit, ensuring that no gap exists between the porous silicon carbide biscuit and the another porous silicon carbide biscuit during jointing, and compacting for a period of time by using a heavy object; and (3) placing the compacted and bonded biscuit in a vacuum sintering furnace, adding sufficient silicon for reaction sintering, and then cleaning the surface to remove residual silicon. The preparation method of the internal defects of the reaction sintering silicon carbide ceramic can accurately prepare design defects with various shapes, and does not introduce other impurities or generate new defects.
Description
Technical Field
The invention relates to the technical field of nondestructive testing, in particular to a preparation method of internal defects of reaction sintered silicon carbide ceramics.
Background
The silicon carbide material has the advantages of high elastic modulus, moderate density, small thermal expansion coefficient, high thermal conductivity coefficient, thermal shock resistance, high specific rigidity, high dimensional stability and the like, so that the silicon carbide material is an ideal selection material for a reflector body of a space optical remote sensor, and is widely applied to preparation of a reflector blank of the space reflector in recent years. The silicon carbide material has many preparation modes, wherein the reaction sintering silicon carbide has the advantages of simple process, short sintering time, low sintering temperature and cost, net-size sintering, easy preparation of large-scale complex-shaped products and the like, so the silicon carbide material becomes the structural ceramic which realizes large-scale industrial application at first and has wide application prospect. However, the generation of defects is unavoidable in actual processing production, while the sensitivity of the ceramic material to defects is much higher than that of materials such as metal, and even the existence of micro defects can easily cause stress concentration at the defects to rapidly cause damage, and especially optical materials have stricter requirements on the quality of products. Therefore, it is very important to control the quality of the product and detect defects.
At present, for silicon carbide materials, which nondestructive testing means is most suitable is not necessarily determined. In order to verify the detection effect of different detection means on the silicon carbide material, the preparation of samples for different types of defects is required. However, the method of directly obtaining the defect sample in the actual production process is not preferable because the size and type of the defect of the sample cannot be accurately judged before detection, and it is relatively difficult to review the detection result. Therefore, it is important to reasonably prepare a silicon carbide defect sample. The main defect preparation method is a mechanical processing method, but the mechanical processing method is not suitable for manufacturing internal defects. And aiming at the nondestructive testing industry, the detection means of the surface defects are various and are easy to realize, the detection of the internal defects is the key point concerned by the nondestructive testing industry, whether the internal defects of the test sample can be efficiently and accurately detected is an important index for evaluating the quality of the nondestructive testing method, and the internal defects of the material can be successfully prepared, so that a research basis is provided for material workers to know the failure condition of the material in use, and the method also has an important propulsion effect on the material detection industry.
Therefore, there is an urgent need to develop a method for preparing internal defects of reaction-sintered silicon carbide ceramic, which can accurately prepare design defects of various shapes, and does not introduce other impurities or generate new defects.
Disclosure of Invention
The invention aims to provide a preparation method of internal defects of reaction sintering silicon carbide ceramics aiming at the defects in the prior art, so that design defects of various shapes can be accurately prepared, other impurities are not introduced, and new defects are not generated.
The object of the invention can be achieved by the following technical measures:
the invention provides a preparation method of internal defects of reaction sintered silicon carbide ceramics, which comprises the following steps:
step 1: preparing two silicon carbide biscuit with same shape and size and flat surface, and then drying and degreasing to obtain porous silicon carbide biscuit;
step 2: coating an inert inorganic substance on the surface of one porous silicon carbide biscuit according to the position of a design defect, and keeping the shape and the size of a forming area coated with the inert inorganic substance consistent with the shape and the size of the design defect to obtain the porous silicon carbide biscuit with prefabricated defects; the inert inorganic substance does not react with silicon and silicon carbide, is not volatilized at high temperature, is not decomposed, and is not wetted by liquid silicon;
and step 3: coating organic binder on the rest positions of the surface of the porous silicon carbide biscuit with the prefabricated defects, flattening the surface of the porous silicon carbide biscuit again, butting and jointing the porous silicon carbide biscuit with another porous silicon carbide biscuit, ensuring that no gap exists between the porous silicon carbide biscuit and the another porous silicon carbide biscuit during jointing, and compacting for a period of time by using a heavy object; the products of the organic binder after pyrolysis have no other solid except carbon, and the rest products do not react with silicon and silicon carbide and are discharged in a gas form;
and 4, step 4: and (3) placing the compacted and bonded biscuit in a vacuum sintering furnace, adding sufficient silicon for reaction sintering, and after sintering, cleaning the surface to remove residual silicon to obtain the silicon carbide ceramic containing internal defects.
Further, the silicon carbide biscuit in the step 1 is prepared through a slip casting or gel casting process, the bending strength of the silicon carbide biscuit is higher than 5MPa, and the flatness of a butt joint binding face of the silicon carbide biscuit is smaller than 0.1 mm.
Further, the inert inorganic substance in the step 2 is any one of zirconium boride, zirconium oxide and silicon dioxide.
Further, the organic binder in step 3 is any one of epoxy resin glue, ethyl cyanoacrylate and polyacrylate.
Furthermore, the bending strength of the bonding part of the biscuit bonded in the step 3 is more than 5 MPa.
Further, the weight in the step 3 enables the pressure on the surface of the load-bearing biscuit to be 4 x 10-3The time is more than 1h between MPa and 1 MPa.
Furthermore, the silicon is added in step 3 in an amount sufficient to fill the pores in the green body after butt bonding and also sufficient to react off carbon generated by pyrolysis of the organic binder.
Furthermore, the adding amount of the silicon in the step 3 is not less than half of the mass of the biscuit after butt joint.
Further, the surface cleaning in the step 4 is in a non-knocking manner.
Further, the surface cleaning in the step 4 is grinding or sand blasting.
The preparation method of the internal defect of the reaction sintering silicon carbide ceramic comprises the steps of bonding two silicon carbide biscuit bodies together by using an organic bonding agent, adding an inert inorganic substance into the biscuit bodies, and using the inert inorganic substance to prevent infiltration of silicon in the biscuit bodies so as to cause silicon area loss and further generate defects. The preparation method of the internal defects of the reaction sintering silicon carbide ceramic is simple and strong in operability, can be used for preparing the internal defects of various shapes to meet the requirements of most non-calculation detection technologies on samples, does not generate the position offset phenomenon of the prefabricated defects in the preparation process, has high accuracy of the prepared internal defects, does not introduce new defects, and provides basic support for development and upgrading of nondestructive detection technologies.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for producing internal defects in reaction-sintered silicon carbide ceramics according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
In order to make the description of the present disclosure more complete and complete, the following description is given for illustrative purposes with respect to the embodiments and examples of the present invention; it is not intended to be the only form in which the embodiments of the invention may be practiced or utilized. The embodiments are intended to cover the features of the various embodiments as well as the method steps and sequences for constructing and operating the embodiments. However, other embodiments may be utilized to achieve the same or equivalent functions and step sequences.
The invention provides a preparation method of internal defects of reaction sintered silicon carbide ceramics, which comprises the following steps as shown in figure 1:
step 1: preparing two silicon carbide biscuit with same shape and size and flat surface, and then drying and degreasing to obtain porous silicon carbide biscuit;
step 2: coating an inert inorganic substance on the surface of one porous silicon carbide biscuit according to the position of a design defect, and keeping the shape and the size of a forming area coated with the inert inorganic substance consistent with the shape and the size of the design defect to obtain the porous silicon carbide biscuit with prefabricated defects; the inert inorganic substance does not react with silicon and silicon carbide, is not volatilized at high temperature, is not decomposed, and is not wetted by liquid silicon;
and step 3: coating organic binder on the rest positions of the surface of the porous silicon carbide biscuit with the prefabricated defects, flattening the surface of the porous silicon carbide biscuit again, butting and jointing the porous silicon carbide biscuit with another porous silicon carbide biscuit, ensuring that no gap exists between the porous silicon carbide biscuit and the another porous silicon carbide biscuit during jointing, and compacting for a period of time by using a heavy object; the products of the organic binder after pyrolysis have no other solid except carbon, and the rest products do not react with silicon and silicon carbide and are discharged in a gas form;
and 4, step 4: and (3) placing the compacted and bonded biscuit in a vacuum sintering furnace, adding sufficient silicon for reaction sintering, and after sintering, cleaning the surface to remove residual silicon to obtain the silicon carbide ceramic containing internal defects.
The silicon carbide biscuit in the step 1 is prepared by a slip casting or gel casting process, and is required to have certain strength, biscuit powder can not fall off due to slight friction, and the bending strength of the silicon carbide biscuit is required to be higher than 5 MPa. And the surface of the silicon carbide is required to be flat, so that excessive concave-convex fluctuation does not exist on the surface of the butt joint binding surface of the silicon carbide biscuit, the glue thickness of a part of binding area is not excessive, and the flatness of the butt joint binding surface of the silicon carbide biscuit is preferably less than 0.1 mm.
Wherein, the inert inorganic substance in the step 2 can be selected from zirconium boride, zirconium oxide, silicon dioxide and the like. The defect size is also reasonably designed to be neither within the minimum size attainable by the inert mineral nor beyond the maximum size of the silicon carbide biscuit.
The organic adhesive in step 3 may be an adhesive such as epoxy resin adhesive, ethyl cyanoacrylate, polyacrylate, or the like, and the bonded portion of the bonded biscuit in step 3 needs to have a certain strength, for example, the bending strength is preferably greater than 5MPa, and the bonded layer is not separated by a slight external force. The time for compacting the weight in step 3 is determined according to the use condition of the organic binder, and the organic binder can be fully acted in the compacting time without influencing the subsequent operation, and the pressure on the surface of the biscuit which is designed to bear the weight is preferably 4 x 10-3The pressure is between MPa and 1MPa, and the compaction time is more than 1 h. In addition, the addition amount of the silicon in the step 3 is enough to fill the holes in the biscuit after butt joint and bonding and also enough to react carbon generated by pyrolysis of the organic binder, and the addition amount of the silicon can be selected to be not less than half of the mass of the biscuit after butt joint and bonding.
The surface cleaning in step 4 is required to be performed in a non-knocking manner, for example, by means of grinding or sand blasting.
Example 1
A preparation method of internal defects of reaction sintered silicon carbide ceramics comprises the following steps:
step 1: preparing a silicon carbide biscuit by adopting a slip casting process, and then drying and degreasing to obtain a porous silicon carbide biscuit; and (4) machining the porous silicon carbide biscuit by using a milling machine to process two samples with the length of 80mm, the width of 40mm and the height of 3.5mm and smooth surfaces.
Step 2: uniformly coating a layer of silica powder with the thickness of about 0.05mm on a central 10mm multiplied by 10mm area of one sample, and uniformly coating the silica powder, alcohol and a small amount of carbon black in advance.
And step 3: the epoxy resin glue is smeared at the rest positions of the sample, the thickness is close to 0.05mm, the thickness can be slightly higher, the condition that the rest positions except the central area are filled with the epoxy resin glue except silicon dioxide is ensured, then the sample is butted and attached with another sample, no gap exists between the two samples when the sample is attached is ensured, the solid iron block is pressed by a 5kg solid iron block, the solid iron block is wrapped by gauze in advance to prevent the sample from being damaged, the whole sample is placed at the backlight position for 24 hours, and the epoxy resin is completely dried.
And 4, step 4: placing the compacted attaching sample in a vacuum sintering furnace, adding silicon according to the amount of 50% of the mass of the sample after bonding, and performing reactive sintering, wherein the sintering control parameters are as follows: heating at the heating rate of 6 ℃/h, keeping the temperature for 2h when the temperature is heated to 1650 ℃, so that the silicon can be completely infiltrated into the biscuit, and cooling to the room temperature at the cooling rate of 6 ℃/h. And after opening the furnace, carrying out sand blasting and polishing treatment on the sample, and cleaning residual silicon on the surface to obtain the silicon carbide ceramic containing internal defects.
The thickness of the test piece was measured by an ultrasonic thickness gauge, and the results showed that the average measured thickness of the center 10mm × 10mm area of the test piece was 3.21mm, and the average measured thickness of the other areas of the test piece was 7.28mm, indicating that the internal defects of the test piece in this example were consistent with the design defects.
Example 2
A preparation method of internal defects of reaction sintered silicon carbide ceramics comprises the following steps:
step 1: preparing a silicon carbide biscuit by adopting a gel casting process, and then drying and degreasing to obtain a porous silicon carbide biscuit; and (4) machining the porous silicon carbide biscuit by using a milling machine to process two samples with the length of 80mm, the width of 40mm and the height of 3.5mm and smooth surfaces.
Step 2: uniformly coating a layer of zirconia powder with the thickness of about 0.05mm on a central 10mm multiplied by 10mm area of one sample, and uniformly coating the silica powder, alcohol and a small amount of carbon black in advance.
And step 3: the epoxy resin glue is smeared at the rest positions of the sample, the thickness is close to 0.05mm, the thickness can be slightly higher, the condition that the rest positions except the central area are filled with the epoxy resin glue except silicon dioxide is ensured, then the sample is butted and attached with another sample, no gap exists between the two samples when the sample is attached is ensured, the solid iron block is pressed by a 5kg solid iron block, the solid iron block is wrapped by gauze in advance to prevent the sample from being damaged, the whole sample is placed at the backlight position for 24 hours, and the epoxy resin is completely dried.
And 4, step 4: placing the compacted attaching sample in a vacuum sintering furnace, adding silicon according to the amount of 50% of the mass of the sample after bonding, and performing reactive sintering, wherein the sintering control parameters are as follows: heating at the heating rate of 6 ℃/h, keeping the temperature for 2h when the temperature is heated to 1650 ℃, so that the silicon can be completely infiltrated into the biscuit, and cooling to the room temperature at the cooling rate of 6 ℃/h. And after opening the furnace, carrying out sand blasting and polishing treatment on the sample, and cleaning residual silicon on the surface to obtain the silicon carbide ceramic containing internal defects.
The thickness of the test piece was measured by an ultrasonic thickness gauge, and the results showed that the average measured thickness of the center 10mm × 10mm area of the test piece was 3.58mm, and the average measured thickness of the other areas of the test piece was 7.28mm, indicating that the internal defects of the test piece in this example were consistent with the design defects.
The preparation method of the internal defect of the reaction sintering silicon carbide ceramic comprises the steps of bonding two silicon carbide biscuit bodies together by using an organic bonding agent, adding an inert inorganic substance into the biscuit bodies, and using the inert inorganic substance to prevent infiltration of silicon in the biscuit bodies so as to cause silicon area loss and further generate defects. The preparation method of the internal defects of the reaction sintering silicon carbide ceramic is simple and strong in operability, can be used for preparing the internal defects of various shapes to meet the requirements of most non-calculation detection technologies on samples, does not generate the position offset phenomenon of the prefabricated defects in the preparation process, has high accuracy of the prepared internal defects, does not introduce new defects, and provides basic support for development and upgrading of nondestructive detection technologies.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of internal defects of reaction sintered silicon carbide ceramic is characterized by comprising the following steps:
step 1: preparing two silicon carbide biscuit with same shape and size and flat surface, and then drying and degreasing to obtain porous silicon carbide biscuit;
step 2: coating an inert inorganic substance on the surface of one porous silicon carbide biscuit according to the position of a design defect, and keeping the shape and the size of a forming area coated with the inert inorganic substance consistent with the shape and the size of the design defect to obtain the porous silicon carbide biscuit with prefabricated defects; the inert inorganic substance does not react with silicon and silicon carbide, is not volatilized at high temperature, is not decomposed, and is not wetted by liquid silicon;
and step 3: coating organic binder on the rest positions of the surface of the porous silicon carbide biscuit with the prefabricated defects, flattening the surface of the porous silicon carbide biscuit again, butting and jointing the porous silicon carbide biscuit with another porous silicon carbide biscuit, ensuring that no gap exists between the porous silicon carbide biscuit and the another porous silicon carbide biscuit during jointing, and compacting for a period of time by using a heavy object; the products of the organic binder after pyrolysis have no other solid except carbon, and the rest products do not react with silicon and silicon carbide and are discharged in a gas form;
and 4, step 4: and (3) placing the compacted and bonded biscuit in a vacuum sintering furnace, adding sufficient silicon for reaction sintering, and after sintering, cleaning the surface to remove residual silicon to obtain the silicon carbide ceramic containing internal defects.
2. The method for preparing internal defects of reaction-sintered silicon carbide ceramic according to claim 1, wherein the silicon carbide green body in the step 1 is prepared by slip casting or gel injection molding, the bending strength of the silicon carbide green body is higher than 5MPa, and the flatness of the abutting joint surface of the silicon carbide green body is less than 0.1 mm.
3. The method for producing internal defects of reaction-sintered silicon carbide ceramic according to claim 1, wherein the inert inorganic substance in the step 2 is any one of zirconium boride, zirconium oxide and silicon dioxide.
4. The method for preparing internal defects of reaction-sintered silicon carbide ceramic according to claim 1, wherein the organic binder in step 3 is any one of epoxy glue, ethyl cyanoacrylate and polyacrylate.
5. The method for producing internal defects in reaction-sintered silicon carbide ceramic according to claim 1, wherein the bending strength of the bonded portion of the joined green body in step 3 is greater than 5 MPa.
6. The method of claim 1, wherein the weight of step 3 subjects the surface of the load-bearing biscuit to a pressure of 4 x 10-3The time is more than 1h between MPa and 1 MPa.
7. The method of claim 1, wherein the silicon is added in an amount sufficient to fill the pores in the butt-bonded green body and to react off carbon generated by pyrolysis of the organic binder in step 3.
8. The method for producing internal defects in reaction-sintered silicon carbide ceramic according to claim 7, wherein the amount of silicon added in step 3 is not less than half of the mass of the biscuit after butt joint.
9. The method for producing internal defects in reaction-sintered silicon carbide ceramic according to claim 1, wherein the surface cleaning in step 4 is performed in a non-tapping manner.
10. The method for producing internal defects in reaction-sintered silicon carbide ceramics according to claim 1, wherein the surface cleaning in step 4 is grinding or sand blasting.
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| CN103641509A (en) * | 2013-12-09 | 2014-03-19 | 中国建筑材料科学研究总院 | Porous carbon preform for reactive sintering, as well as preparation method and application thereof |
| CN103737190A (en) * | 2014-01-02 | 2014-04-23 | 江苏大学 | Method for prefabricating hole type weld defect |
| CN104931320A (en) * | 2015-06-24 | 2015-09-23 | 桂林电子科技大学 | Sample piece with two material interfaces containing preset microcracks and production method of sample piece |
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