CN111089774A - Surface corrosion treatment method of boron carbide product, metallographic sample and preparation method of metallographic sample - Google Patents
Surface corrosion treatment method of boron carbide product, metallographic sample and preparation method of metallographic sample Download PDFInfo
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- CN111089774A CN111089774A CN201910982610.9A CN201910982610A CN111089774A CN 111089774 A CN111089774 A CN 111089774A CN 201910982610 A CN201910982610 A CN 201910982610A CN 111089774 A CN111089774 A CN 111089774A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
Abstract
The invention relates to a surface corrosion treatment method of a boron carbide product, a boron carbide metallographic specimen and a preparation method thereof. The surface corrosion treatment method comprises the following steps: enabling the temperature of a boron carbide product to be treated to be at a preset temperature, and corroding the boron carbide product by using a first corrosive agent at a first temperature for a first preset time, wherein the preset temperature is higher than room temperature and lower than the first temperature; cooling the boron carbide product after corrosion treatment is obtained, and carrying out corrosion treatment on the boron carbide product at a second temperature for a second preset time which is not less than the first preset time by using a second corrosive agent, wherein the second corrosive agent is different from the first corrosive agent, and the second temperature is lower than the preset temperature; after obtaining the boron carbide product subjected to corrosion treatment, carrying out corrosion treatment on the boron carbide product at a third temperature for a third preset time which is not more than the first preset time by using a third corrosive agent, wherein the third corrosive agent is different from the second corrosive agent, and the third temperature is not lower than the first temperature; obtaining the boron carbide product after corrosion treatment and cooling the boron carbide product.
Description
Technical Field
The invention relates to the field of boron carbide product process treatment, in particular to a surface corrosion treatment method of a boron carbide product, a preparation method of a boron carbide metallographic specimen and the boron carbide metallographic specimen.
Background
Due to the material properties of boron carbide itself, e.g., in terms of hardness, numerous types of boron carbide articles have been provided. For example, in the case of boron carbide ceramics, the application of surface microstructure morphology analysis is a conventional detection means for characterizing the boron carbide ceramics according to relevant standards and regulations, and pores, grain size, grain shape, grain boundaries and the like of the corroded boron carbide ceramics can be observed through the microstructure. The boron carbide ceramic is a compact ceramic sintered by submicron-grade boron carbide powder, adding a small amount of Si and B as sintering aids, and applying a certain pressure at 1800-1900 ℃ under the inert atmosphere or vacuum condition. The boron carbide ceramic has good chemical stability, and methods such as chemical corrosion, ion etching and the like are generally adopted to observe the microscopic morphology of the boron carbide ceramic. However, these prior methods still suffer from several drawbacks and deficiencies. For example, in a common chemical etching method, a single acid or alkali is used for etching, which often causes problems of incomplete and unclear etching interface, excessive etching and the like due to an unobvious etching effect and damage to the morphology of crystal grains or crystal boundaries. For another example, the ion etching method is to remove the surface of the ceramic by using high-energy ions, but in the etching process, since the high-energy ions are easy to introduce new defects and the grain boundary of the etched ceramic sample is unclear, the preparation of the etching solution, the etching temperature and the etching time are all important and difficult to operate and control in order to observe clear grains and grain boundaries.
It should be noted that what is described in this section relates to corresponding research and understanding by the inventors and, therefore, should not be taken to be prior art or to be obvious merely because it is included in this section.
Disclosure of Invention
In view of the above, the present invention provides a method for surface corrosion treatment of a boron carbide article, a method for preparing a boron carbide metallographic specimen, and a boron carbide metallographic specimen, which can solve or at least alleviate one or more of the above-mentioned problems and other problems of the prior art.
First, according to a first aspect of the present invention, there is provided a surface etching treatment method for a boron carbide article, comprising the steps of:
A. enabling the temperature of a boron carbide product to be treated to be at a preset temperature, and corroding the boron carbide product at a first temperature and a first preset time length by using a first corrosive agent, wherein the preset temperature is higher than the room temperature and lower than the first temperature;
B. cooling the boron carbide product subjected to corrosion treatment after obtaining the boron carbide product, and performing corrosion treatment on the boron carbide product at a second temperature for a second preset time which is not less than the first preset time by using a second corrosive agent, wherein the second corrosive agent is different from the first corrosive agent, and the second temperature is lower than the preset temperature;
C. after obtaining the boron carbide product subjected to corrosion treatment, carrying out corrosion treatment on the boron carbide product at a third temperature for a third preset time which is not more than the first preset time by using a third corrosive agent, wherein the third corrosive agent is different from the second corrosive agent, and the third temperature is not lower than the first temperature; and
D. obtaining the boron carbide product after corrosion treatment and cooling the boron carbide product.
In the surface corrosion treatment method of a boron carbide article according to the present invention, optionally, the surface corrosion treatment method further includes the steps of: in the step B, the step C and/or the step D, after the boron carbide product subjected to corrosion treatment is obtained, cleaning treatment is carried out on the boron carbide product by using at least one cleaning liquid.
In the surface corrosion treatment method of a boron carbide article according to the present invention, optionally, the cleaning treatment includes: and cleaning the boron carbide product at least twice by using a first cleaning solution, and cleaning the boron carbide product at least once by using a second cleaning solution in the process, wherein the first cleaning solution comprises ionized water, and the second cleaning solution comprises alcohol.
In the surface corrosion treatment method of a boron carbide article according to the present invention, optionally, the surface corrosion treatment method further includes the steps of: and keeping the cleaned boron carbide product at a preset temperature for a preset time, wherein the preset temperature ranges from 90 ℃ to 130 ℃, and the preset time ranges from 10 minutes to 30 minutes.
In the surface etching treatment method of a boron carbide article according to the present invention, optionally, the first etchant and the third etchant are the same or different alkaline solutions, and the second etchant is an acidic solution; and/or
The preset temperature range is 150-.
In the surface etching treatment method of a boron carbide product according to the present invention, optionally, the first etchant and/or the third etchant is a solution prepared by mixing sodium hydroxide having a mass purity of not less than 99% with water, and/or the second etchant is hydrochloric acid having a concentration in a range of 25 to 35%.
In the method for treating the surface of the boron carbide product by corrosion according to the present invention, optionally, in step a, the surface roughness Ra of the boron carbide product to be treated is not greater than 0.2um, the temperature of the boron carbide product is raised from room temperature to a first preset temperature and is maintained for a first preset time period, and then the temperature of the boron carbide product is raised to the preset temperature and is maintained for a second preset time period according to a first preset temperature raising rate; and/or raising the temperature of the first corrosive agent from room temperature to a second preset temperature which is not higher than the first temperature according to a second preset raising rate and keeping the temperature for a third preset time.
In the method for surface corrosion treatment of a boron carbide product according to the present invention, optionally, the first preset temperature is in the range of 90-150 ℃ and/or the first preset time period is in the range of 30-90 minutes and/or the second preset temperature is in the range of 300-400 ℃ and/or the second preset time period is in the range of 10-50 minutes and/or the first preset temperature rise rate is in the range of 0.5-1.5 ℃/min and/or the second preset temperature rise rate is in the range of 0.5-1.5 ℃/min and/or the third preset time period is in the range of 1-3 hours.
Secondly, according to a second aspect of the present invention, there is provided a method for preparing a boron carbide metallographic specimen, comprising the steps of:
providing a sample at least the surface of which is provided with a boron carbide material layer; and
treating the sample by using the surface corrosion treatment method of the boron carbide product as described in any one of the above to prepare a boron carbide metallographic sample for observing a metallographic microstructure.
Furthermore, according to the third aspect of the present invention, there is also provided a boron carbide metallographic specimen prepared by using the method for preparing a boron carbide metallographic specimen as described above.
The principles, features, characteristics, advantages and the like of various aspects according to the present invention will be clearly understood from the following detailed description taken in conjunction with the accompanying drawings. For example, it will be understood that, compared with the prior art, the technical scheme of the invention can safely and effectively corrode the crystal phase organization structure of the boron carbide surface, the crystal boundary after corrosion is complete and clear, the crystal grain contrast is obvious, and the defects of surface morphology damage and the like caused by other methods can be effectively avoided, so that the surface structure, the crystal grain size and distribution, the air holes and impurity phase distribution and the like can be clearly observed, the microstructure morphology of the boron carbide product to be prepared can be accurately obtained, the material performance can be accurately evaluated, and a powerful basis is provided for the improvement of the next product preparation process.
Drawings
The present invention will be described in further detail below with reference to the drawings and examples, but it should be understood that the drawings are designed solely for purposes of illustration and are not necessarily drawn to scale, but rather are intended to conceptually illustrate the structural configurations described herein.
FIG. 1 is a process flow diagram of an embodiment of a method for treating the surface of a boron carbide article by etching in accordance with the present invention.
FIG. 2 is a microstructure observed after a boron carbide ceramic article has been surface etched using an embodiment of the method of surface etching according to the present invention.
FIG. 3 is a process flow diagram of one embodiment of a method for preparing a boron carbide metallographic specimen of a boron carbide article according to the invention.
Detailed Description
It should be noted that the surface corrosion treatment method of the boron carbide product, the preparation method of the boron carbide metallographic specimen, the steps, the characteristics, the advantages and the like of the boron carbide metallographic specimen according to the present invention will be described below by way of example, but all the descriptions should not be construed to limit the present invention in any way. It should also be noted that, for any single feature described or implicit in the embodiments referred to herein, the invention still allows any combination or permutation to be continued between these features (or their equivalents) without any technical hurdle, so that further embodiments according to the invention should be considered within the scope of this description.
In addition, as used herein, the technical phrase "boron carbide article" refers to an article that is made using, consists essentially of, or consists of a portion of a boron carbide material, and the technical terms "first", "second", and "third" are used for descriptive purposes only and are not intended to indicate their sequential or relative importance. Moreover, any reference herein to any given value shall be understood to also encompass insubstantial errors associated with its measurement, e.g., ranges of ± 8%, ± 5%, or ± 2%, etc., of the given value.
First, fig. 1 shows a basic process flow of an embodiment of the method for surface-etching a boron carbide article according to the present invention, which can be used to surface-etch many types of boron carbide articles, such as boron carbide ceramic samples, according to the application requirements. By way of illustration, in the example given in fig. 1, the surface corrosion treatment method may include the steps of:
first, in step S11, a boron carbide article to be treated is prepared, and such boron carbide article may have any possible shape configuration, such as a rod shape, a rectangular parallelepiped shape, a spherical shape, or the like. In order to further facilitate the surface treatment of the boron carbide product in the subsequent process steps, it is considered to provide the boron carbide product with a smooth surface meeting the set requirements, for example, at least a part of the surface can reach the surface roughness Ra of not more than 0.2um by any possible process method such as polishing, grinding, etc., and the specific requirements can be selected and set according to the requirements of the implementation application.
As shown in FIG. 1, the prepared boron carbide article may be heated to a predetermined temperature, for example, between 150 ℃ and 250 ℃, which may be accomplished in a variety of ways. By way of example only, the boron carbide article may be initially placed in an apparatus such as an oven to be raised from room temperature to a predetermined temperature (e.g., 110 ℃ or other suitable value) and held for a predetermined period of time (e.g., 30-90 minutes or other suitable value), and then the temperature of the boron carbide article may be gradually and steadily raised to a higher predetermined temperature at a predetermined ramp rate (e.g., 0.5-1.5 ℃/min or other suitable value), which may be accomplished, for example, by operating a ramp control device in a muffle or other electric furnace, and held at the higher temperature for a predetermined period of time (e.g., 10-50 minutes or other suitable value). The boron carbide article may then be subjected to a first etching process, for example, using a clean crucible tongs or the like, by being fed into a first etchant as will be described below.
The first etchant is provided to etch the boron carbide article and may be any suitable etchant solution, such as alkaline, acidic, and the like. By way of example, a sodium hydroxide solution may be employed in this embodiment. Specifically, for example, sodium hydroxide powder having a mass purity of not less than 99% may be added to a suitable container such as a nickel metal reaction container, and may be added in a ratio of one-half of the container volume or other ratios according to specific requirements to be mixed with water to form a caustic sodium hydroxide solution. The vessel is then placed in an apparatus such as a muffle furnace for heating and may be raised from room temperature to a predetermined temperature (e.g., 300 ℃ to 400 ℃ or other suitable value which is not greater than the first temperature as described below) at a predetermined ramp rate (e.g., 0.5 to 1.5 ℃/min or other suitable value) and held at that temperature for a predetermined period of time (e.g., 1 to 3 hours or other suitable value) at which the sodium hydroxide solution may be in a molten state.
After the sodium hydroxide solution in the above state is contacted with the boron carbide product, it will perform a rapid corrosion treatment on the surface of the boron carbide product, and the working temperature at this time can be controlled at a first temperature (e.g. 350-.
Next, in step S12, the boron carbide product after the above etching treatment may be taken out from the sodium hydroxide solution and cooled, and for example, natural cooling, air cooling, or other feasible methods may be employed. The boron carbide article may then be continued to be etched using a second etchant, different from the sodium hydroxide solution described above. For example, the second etchant may be a suitable acidic solution such as hydrochloric acid, for example, concentrated hydrochloric acid having a concentration ranging from 25% to 35% may be used to etch the boron carbide article, thereby forming a cross-corrosion effect on the surface of the boron carbide article together with the above-mentioned sodium hydroxide solution, because the molten sodium hydroxide solution may dissolve boron carbide, which may form corrosion defects on the surface of the boron carbide article when used alone, while hydrochloric acid has a dual effect of being neutralized with the sodium hydroxide solution and performing a corrosion treatment on the boron carbide, and thus may be used to slowly neutralize the sodium hydroxide solution and slowly corrode at grain boundaries of the boron carbide article to form complete and clear grain boundaries, which is not at all possible using prior art methods. Therefore, the microstructure structure of the crystal phase on the surface of the boron carbide can be safely and effectively corroded and exposed, so that the microstructure structure with the compact boron carbide ceramic surface can be clearly observed and analyzed, a worker can be prompted to accurately know the size and distribution of crystal grains, the distribution of air holes and impurity phases and the like, and a reliable basis can be provided for the implementation of process improvement and other aspects.
In actual use, the second etchant described above may be used to perform the second etching treatment on the boron carbide product at the second temperature (e.g., room temperature or other higher temperature value), and the etching treatment time may be set to be maintained for a preset time period, such as 1-4 hours or other suitable value, and the time period may be no less than the time spent in etching the boron carbide product by using the first etchant.
Next, in step S13, the boron carbide product after the second etching treatment may be taken out of the second etchant, and then the etching treatment may be continued on the boron carbide product using the third etchant, that is, the third etching treatment may be performed. Specifically, the third etchant may be a first etchant (for example, the above-mentioned sodium hydroxide solution) as it is, or may be another etchant different from the first etchant, for example, another alkaline etchant or an isotropic etchant having a concentration different from that of the first etchant. In practical applications, the third etchant may be subjected to an etching reaction with the boron carbide product at a third temperature (e.g., 500 ℃. & 700 ℃ or other suitable temperature value), and the etching treatment time may be set to be maintained for a predetermined period of time, e.g., 1-10 minutes or other suitable value, so as to obtain the boron carbide product after further surface etching treatment.
In this way, after the boron carbide product subjected to the third etching treatment is obtained in step S14, the boron carbide product may be cooled by using available methods such as natural cooling and air cooling, so as to obtain the desired metallographic structure of the boron carbide product after the surface etching has been completed.
The above description has been given by way of example only to a general description of the method for the treatment of the surface of a boron carbide article by etching, but it should be understood that the present invention allows any possible variation, modification or adaptation, etc., according to the requirements of different applications.
For example, as an alternative, after the boron carbide article is subjected to the first, second, and/or third etching treatment described above, the boron carbide article after the etching treatment is completed may be subjected to a cleaning treatment using one or more cleaning liquids. For example, the boron carbide product after the etching treatment may be cleaned twice or more with one cleaning solution (e.g., ionized water, etc.), and the boron carbide product may be cleaned again with another cleaning solution (e.g., alcohol, etc.) therebetween, and their respective specific cleaning operation durations may be flexibly set or adjusted according to the needs, for example, each cleaning operation may be performed for 10 seconds, 20 seconds, etc., and the cleaning operation durations of different times may be the same or different from each other. In addition, after the first and/or third etching treatment, boiled dilute hydrochloric acid can be optionally used as a cleaning solution to clean and remove the sodium hydroxide solution attached to the boron carbide product.
For another example, in an alternative embodiment, the cleaned boron carbide article may be maintained at a predetermined temperature for a predetermined period of time so that it may be maintained in a dry state to facilitate further processing operations. By way of illustration, the respective ranges of the predetermined temperature and the predetermined time may be 90-130 ℃ and 10-30 minutes, and the specific value setting may be selected or adjusted according to the actual application requirement.
For another example, in the foregoing embodiment, the first etchant and the third etchant use alkaline solutions, and the second etchant uses acidic solutions, so that the acid-base cross-etching treatment can be performed on the surface of the boron carbide product. However, in some embodiments, it is also contemplated that the first etchant and the third etchant may be selected from acidic solutions, and the second etchant may be selected from basic solutions, which may also result in an acid-base cross-etching treatment. Of course, in other embodiments, the present invention also allows the use of various other possible corrosive solutions for each of the above etchants, depending on the particular application.
The method for treating the surface of the boron carbide product by corrosion is further described with reference to the metallographic picture example shown in fig. 2, so that the technical scheme of the invention and the outstanding advantages of the method over other methods in the prior art can be more completely and clearly understood.
Referring to fig. 2, in the figure, the microstructure of the boron carbide ceramic product observed under a high power metallographic microscope is obtained after a boron carbide ceramic product is subjected to corrosion treatment in a sodium hydroxide solution in a molten state of 350-500 ℃ for 20 minutes, then is subjected to corrosion treatment with concentrated hydrochloric acid for 2 hours, and then is subjected to corrosion treatment in a sodium hydroxide solution in a molten state of 500-900 ℃ for 5 minutes, and it can be seen from fig. 2 that the metallographic microstructure has very clear grain boundaries, the grains are complete and clear, the grain contrast is obvious, and no obvious corrosion defects exist.
According to another technical scheme, the invention also provides a preparation method of the boron carbide metallographic sample, wherein the surface corrosion treatment method of the boron carbide product designed and provided according to the invention is used, so that the obvious technical advantages of the scheme of the invention compared with other methods in the prior art can be exerted. For example, the preparation method of the boron carbide metallographic specimen can comprise the following steps:
first, in step S21, a sample of a gold boron carbide article is provided, which may be made entirely of a boron carbide material, or may be made substantially of a boron carbide material (e.g., containing unavoidable impurities or other non-primary components), or may be formed with a layer of boron carbide material only on the surface of the sample (i.e., the substrate of the sample may be made of other materials than boron carbide), all of which are suitable for etching using the method of the present invention.
Then, in step S22, the surface corrosion treatment method provided by the present invention can be used to perform corrosion treatment on the sample, so that a boron carbide metallographic sample that can be used to observe the metallographic microstructure can be prepared.
In addition, according to an technical scheme of the invention, the invention also provides a boron carbide metallographic specimen which is prepared by using the preparation method of the boron carbide metallographic specimen designed according to the invention. By providing the boron carbide metallographic specimen, the crystal boundary is complete and clear, the grain contrast is obvious, and the defects caused by the fact that the shape is damaged by corrosive liquid and high-energy etching in other methods in the prior art can be effectively avoided, so that the microstructure shape of the boron carbide product to be prepared can be accurately obtained, the performance of the material can be conveniently and accurately evaluated, and the method is very helpful for providing improvement basis for the preparation process of the product and the like.
The surface corrosion treatment method of a boron carbide article, the preparation method of a boron carbide metallographic specimen and the boron carbide metallographic specimen according to the present invention have been explained in detail above by way of examples only, and these examples are only for illustrating the principle of the present invention and the embodiments thereof, and are not intended to limit the present invention, and various modifications and improvements can be made by those skilled in the art without departing from the spirit and scope of the present invention. Accordingly, all equivalents are intended to be included within the scope of this invention and defined in the claims which follow.
Claims (10)
1. A surface corrosion treatment method of a boron carbide product is characterized by comprising the following steps:
A. enabling the temperature of a boron carbide product to be treated to be at a preset temperature, and corroding the boron carbide product at a first temperature and a first preset time length by using a first corrosive agent, wherein the preset temperature is higher than the room temperature and lower than the first temperature;
B. cooling the boron carbide product subjected to corrosion treatment after obtaining the boron carbide product, and performing corrosion treatment on the boron carbide product at a second temperature for a second preset time which is not less than the first preset time by using a second corrosive agent, wherein the second corrosive agent is different from the first corrosive agent, and the second temperature is lower than the preset temperature;
C. after obtaining the boron carbide product subjected to corrosion treatment, carrying out corrosion treatment on the boron carbide product at a third temperature for a third preset time which is not more than the first preset time by using a third corrosive agent, wherein the third corrosive agent is different from the second corrosive agent, and the third temperature is not lower than the first temperature; and
D. obtaining the boron carbide product after corrosion treatment and cooling the boron carbide product.
2. The surface corrosion treatment method of a boron carbide article according to claim 1, further comprising the steps of: in the step B, the step C and/or the step D, after the boron carbide product subjected to corrosion treatment is obtained, cleaning treatment is carried out on the boron carbide product by using at least one cleaning liquid.
3. The surface corrosion treatment method of a boron carbide article according to claim 2, wherein the cleaning treatment comprises: and cleaning the boron carbide product at least twice by using a first cleaning solution, and cleaning the boron carbide product at least once by using a second cleaning solution in the process, wherein the first cleaning solution comprises ionized water, and the second cleaning solution comprises alcohol.
4. The surface corrosion treatment method of a boron carbide article according to claim 2, further comprising the steps of: and keeping the boron carbide product subjected to the cleaning treatment at a preset temperature for a preset time, wherein the preset temperature is in a range of 90-130 ℃, and the preset time is in a range of 10-30 minutes.
5. The surface etching treatment method of a boron carbide article according to any one of claims 1 to 4, wherein the first etchant and the third etchant are the same or different alkaline solutions, and the second etchant is an acidic solution; and/or
The preset temperature range is 150-.
6. The surface etching treatment method for a boron carbide product according to claim 5, wherein the first etchant and/or the third etchant is a solution prepared by mixing sodium hydroxide having a purity of not less than 99% by mass with water, and/or the second etchant is hydrochloric acid having a concentration ranging from 25% to 35%.
7. The surface corrosion treatment method of a boron carbide product according to any one of claims 1 to 4, wherein in the step A, the surface roughness Ra of the boron carbide product to be treated is not more than 0.2um, the temperature of the boron carbide product is raised from room temperature to a first preset temperature and is kept for a first preset time period, and then the temperature of the boron carbide product is raised to the preset temperature and is kept for a second preset time period according to a first preset temperature raising rate; and/or raising the temperature of the first corrosive agent from room temperature to a second preset temperature which is not higher than the first temperature according to a second preset raising rate and keeping the temperature for a third preset time.
8. The method for surface corrosion treatment of a boron carbide article according to claim 7, wherein the first predetermined temperature is in the range of 90-150 ℃ and/or the first predetermined period of time is in the range of 30-90 minutes and/or the second predetermined temperature is in the range of 300-400 ℃ and/or the second predetermined period of time is in the range of 10-50 minutes and/or the first predetermined ramp rate is in the range of 0.5-1.5 ℃/min and/or the second predetermined ramp rate is in the range of 0.5-1.5 ℃/min and/or the third predetermined period of time is in the range of 1-3 hours.
9. The preparation method of the boron carbide metallographic specimen is characterized by comprising the following steps of:
providing a sample at least the surface of which is provided with a boron carbide material layer; and
treating the sample by using the surface corrosion treatment method of the boron carbide product as set forth in any one of claims 1 to 8, thereby preparing a metallographic sample of boron carbide for observing the metallographic microstructure.
10. A boron carbide metallographic specimen prepared by the method for preparing a boron carbide metallographic specimen according to claim 9.
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| CN116773311A (en) * | 2023-06-26 | 2023-09-19 | 陕西长羽航空装备股份有限公司 | Multistage corrosion method of deformed superalloy material for aeroengine part test |
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