CN111795984B - Sample preparation method for observing microstructure inside ceramic by scanning electron microscope - Google Patents
Sample preparation method for observing microstructure inside ceramic by scanning electron microscope Download PDFInfo
- Publication number
- CN111795984B CN111795984B CN202010573950.9A CN202010573950A CN111795984B CN 111795984 B CN111795984 B CN 111795984B CN 202010573950 A CN202010573950 A CN 202010573950A CN 111795984 B CN111795984 B CN 111795984B
- Authority
- CN
- China
- Prior art keywords
- ceramic
- sample
- scanning electron
- electron microscope
- submicron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a sample preparation method for observing the microstructure in ceramics by a scanning electron microscope, which comprises the steps of breaking a ceramic sample with submicron crystal grains to obtain a fresh section, and performing thermal corrosion or acid corrosion to obtain a ceramic material to be observed; the ceramic sample with submicron-sized grains breaks in a complete or partial transgranular fracture mode.
Description
Technical Field
The invention relates to a sample preparation method for observing a microstructure in a ceramic by a scanning electron microscope, in particular to a preparation method of a scanning electron microscope sample of a ceramic material with submicron crystal grains, belonging to the technical field of material test and analysis.
Background
The shape, size, distribution and the like of crystal grains of the ceramic material can obviously influence the performance of the aspects of mechanics, optics, electricity and the like of the material, so that the clear imaging of the microstructure of the ceramic material is the premise for representing the microscopic characteristics of the ceramic. At present, there are two widely used methods for observing the internal microstructure of a ceramic material by a scanning electron microscope, one is direct section observation, and the other is observation after corroding a polished surface.
Firstly, the method of directly observing the microstructure on the cross section is adopted, the observation result is influenced by the fracture mode of the material, and the universality is not high. The ceramic material fractured along the crystal has obvious fracture surface crystal grains under a scanning electron microscope and clearer crystal boundary, and can meet the observation requirement; however, the ceramic material which is broken by transgranular fracture has flat fracture surface and no contrast between crystal grains and crystal boundaries, and cannot meet the observation requirement.
The sample preparation method of the corrosion polished surface is adopted, particularly for the ceramics with submicron crystal grains, precise polishing equipment and abundant polishing experience are needed, the process is complex, time is consumed, the cost is high, and even the polishing process is difficult to realize; secondly, the real surface of the ceramic material is damaged in the polishing process, local grains are stripped and fall off under the action of mechanical force, and particles in the polishing solution are also remained on the surface of the sample, so that the microstructure inside the sample is distorted; in addition, the surface energy of a sample treated by the polishing process is reduced, and a grain boundary area is more stable, so that greater difficulty is brought to a corrosion process, the corrosion condition is unstable, and the equipment cost and the time cost are increased.
In summary, the first method of directly observing the fracture surface in two methods of observing the microstructure inside the ceramic material by a scanning electron microscope in the prior common knowledge is poor in universality and is not suitable for ceramic samples which are completely transcrystallized and fractured and ceramic samples which are partially transcrystallized and fractured; the second method for corroding the polished surface has complex process flow, redundancy and high uncertainty, and is difficult to realize the requirements of rapid, convenient and accurate sample preparation.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a rapid and simple sample preparation method for observing the internal microstructure of the ceramic by a scanning electron microscope aiming at a ceramic sample with complete crystal-crossing fracture and a ceramic sample with partial crystal-crossing fracture, so that a ceramic material to be observed is obtained after the ceramic sample with submicron crystal grains is fractured to obtain a fresh section and then is subjected to thermal corrosion or acid corrosion; the ceramic sample with submicron-sized grains breaks in a complete or partial transgranular break.
In the disclosure, a fresh section formed by directly breaking a submicron crystal grain ceramic sample is found for the first time, and the roughness generated on a broken surface by the height difference of a plurality of submicron crystal grains is still in the submicron order, so that the roughness of the obtained fresh section is small in an area containing a certain number of crystal grains, the fresh section is flat, the polishing step is not needed, and after direct hot corrosion or acid corrosion, the fresh section can be used for observing and obtaining excellent crystal grains, crystal grain boundaries and other microscopic appearances, and the problem that no contrast or low contrast exists between the crystal grains in a crystal-passing broken surface during direct observation is avoided.
In the present invention, the ceramic having submicron-sized grains has an average grain size of < 5 μm, and preferably, an average grain size of < 1 μm. When the crystal grains are finer, the area containing a certain number of crystal grains on the fresh section is smoother, and clear imaging of the observation area is facilitated.
In the present invention, the ceramic samples include dense ceramics and porous ceramics.
In the invention, the relative density of the compact ceramic is more than 65%; the porous ceramic consists of a pore region without crystal grains and a non-pore framework region with crystal grains, and the relative density of the non-pore framework region is more than 65 percent. In the actual observation process, the porous ceramics are observed, and a non-porous skeleton region is generally observed.
In the invention, the ceramic sample comprises oxide ceramics such as magnesium aluminate spinel, alumina and zirconia and non-oxide ceramics such as aluminum nitride, silicon carbide and boron nitride.
In the invention, the temperature of the hot corrosion is 100-500 ℃ lower than the sintering temperature of the ceramic sample, and under the temperature, the effective corrosion of a grain boundary phase can be realized, so that the contrast between a grain boundary and grains is obvious, the grains can be prevented from growing again, and the original microstructure is kept.
In the invention, the hot corrosion time is 0.5-10 hours. And the time of the hot corrosion is the target temperature heat preservation time, and the time required by the heating process of the heating equipment is not calculated in the hot corrosion time.
In the invention, the acid used in the acid corrosion process is a strong acid solution, preferably at least one selected from a hydrochloric acid solution, a sulfuric acid solution, a nitric acid solution and a phosphoric acid solution; the concentration of the strong acid solution is 1-25 mol/L.
In the invention, the temperature of the acid corrosion is 15-300 ℃, and the time is 1 second-60 minutes.
In the invention, the surface of the obtained ceramic material to be observed is subjected to film coating treatment; the film is made of gold, chromium or carbon, and the thickness of the film is less than or equal to 10 nm. Since the conductivity of the ceramic material to be observed is relatively poor, the ceramic material needs to be subjected to a plating treatment to improve the conductivity, but the thickness of the ceramic material is generally in the nm order so as not to affect the observation of the grain boundary of the ceramic grains and the like. It should be noted that there are low voltage scanning electron microscopes in the field, which may not be coated with a film and also meet the requirements for scanning electron microscope observation.
In another aspect, the present invention also provides a ceramic material to be observed prepared according to the above-described sample preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1. the method does not relate to the technical processes of grinding, polishing and the like, simplifies the technical steps, greatly shortens the sample preparation time and reduces the cost brought by the polishing process;
2. according to the method, the ceramic sample is prepared by corroding the section of the ceramic sample, so that the original morphological characteristics of the sample are kept, small grains are prevented from being peeled off in the polishing process, and misjudgment of the residual particles in the polishing solution on the observation of a scanning electron microscope is avoided;
3. the method has the advantages of stable corrosion condition, no influence of the polishing process on the corrosion condition, simplified operation process, saved sample preparation time and reduced cost.
Drawings
FIG. 1 is a scanning electron microscope image of a hot-etched cross section of a submicron-grained magnesium aluminate spinel ceramic prepared in example 1;
FIG. 2 is a scanning electron micrograph of a fresh cross section of a micron-grained magnesia alumina spinel ceramic made according to example 1;
FIG. 3 is a scanning electron micrograph of a hot-etched cross-section of the 85% relative density alumina ceramic prepared in example 2;
FIG. 4 is a scanning electron micrograph of an acid etched cross section of a 95% relative density alumina ceramic prepared in example 3;
FIG. 5 is a scanning electron micrograph of a cross section of 95% relative density alumina ceramic prepared in example 3;
FIG. 6 is a scanning electron micrograph of a cross-sectional hot corrosion of the 99.99% relative density zirconia ceramic prepared in example 4.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
The method is a brand-new sample preparation method for observing the internal microstructure of the ceramic by using a scanning electron microscope, does not need any precision machining processes such as grinding or polishing, and can realize clear observation on the microscopic features such as crystal grains, pores and crystal boundaries of the ceramic with submicron crystal grains only by combining a simply-made ceramic fracture (fresh section) with a specific corrosion method.
Compared with the widely used sample preparation method for corroding the polished surface, the sample preparation method for observing the microstructure in the ceramic by using the scanning electron microscope provided by the invention does not need a polishing process, and simplifies the process; the damage to the internal microstructure of the ceramic material in the polishing process is avoided, and a more real internal microstructure of the ceramic can be reduced; the corrosion condition is stable and can not generate obvious change along with the change of the sintering temperature of the sample. In general, the fracture mode of the ceramic sample is not only influenced by the kind of material, but may also cause the fracture mode to vary depending on the preparation method. In the field, (1) for submicron crystal ceramics which are completely fractured along the crystal, a method for observing a fresh section is directly adopted, so that a good microscopic morphology picture can be obtained; (2) for submicron grain ceramics which are completely transgranular and fractured or partially transgranular and fractured, a good micro-morphology picture can be obtained by adopting the method for corroding the fresh section.
The following is an exemplary description of a sample preparation method for observing the internal microstructure of the ceramic by scanning electron microscopy.
The ceramic samples are selected such that their relative density is greater than 65% and the grain size is less than 5 μm, and they fracture in a fully transgranular fracture mode or in a partially transgranular fracture mode. Preferably, the grain size of the ceramic sample is < 1 μm. In the present invention, ceramic samples having submicron-sized grains can be purchased directly. Or the ceramic sample with submicron crystal grains is prepared by adjusting parameters such as a forming method, sintering temperature, time and the like in the existing ceramic preparation method. For example, after the raw material powder is formed by a specific forming method and sintered at high temperature, the relative density of a compact non-porous area of the obtained ceramic sample is more than 65%, and at the moment, the ceramic crystal grains and the crystal boundary are formed, the grain size is less than 5 μm, and the preferred grain size is less than 1 μm. The components of the selected ceramic sample include, but are not limited to, oxide ceramics such as magnesium aluminate spinel, zirconia, alumina, etc., and non-oxide ceramics such as aluminum nitride, silicon carbide, boron nitride, etc.
And breaking the ceramic sample to be observed, and taking the fresh and clean section as a surface to be observed, namely a fresh section. The ceramic sample can be broken or chipped to obtain a fresh fracture surface, typically using simple hardware such as pliers or a hammer.
And (6) corrosion. And carrying out hot corrosion or acid corrosion on the obtained ceramic sample, so that the contrast between the grain boundary and the crystal grain is obvious.
In an alternative embodiment, the hot etching may be performed in a muffle furnace, the temperature of which depends on the composition of the ceramic sample. The temperature of the hot corrosion is lower than the sintering temperature of the ceramic sample, and is generally 100-500 ℃ lower. The time for the hot etching may be 0.5 to 10 hours.
In an alternative embodiment, the acid etching conditions are dependent on the composition of the ceramic sample, and the acid selected may not be corrosive to the ceramic grains. The acid solution used in the acid etching can be strong acid such as hydrochloric acid, sulfuric acid, phosphoric acid, etc., and the concentration is generally distributed in the range of 1-25 mol/L. The treatment temperature of the acid corrosion is 15-300 ℃, and the time can be 1 second-60 minutes.
In an alternative embodiment, the surface of the ceramic material to be observed is subjected to a coating treatment, and the existing methods such as magnetron sputtering and evaporation can be adopted to enhance the conductivity. The material of the film can be gold, chromium or carbon, etc., and the thickness is generally in nm level.
And finally, observing the microstructure of the prepared sample by using a scanning electron microscope, and photographing and recording the appearance of the obtained section.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1: scanning electron microscope image of hot corrosion section of prepared magnesia-alumina spinel ceramic
Preparing a ceramic biscuit with a relative density of 56% by using commercial magnesium aluminate spinel powder as a raw material by adopting a gel casting method, and sintering for 6 hours at 1500 ℃ in an air atmosphere to obtain magnesium aluminate spinel ceramic with a relative density of 93%;
breaking the obtained magnesia-alumina spinel ceramic, taking a fresh and clean section as a sample, wherein the microstructure of the fresh section is shown in figure 2, as can be seen from the figure, no lining exists between crystal grains and a crystal boundary, and the ceramic sample is broken in a transgranular breaking mode;
placing the sample in a muffle furnace for hot corrosion, controlling the corrosion temperature to be 1200 ℃, and keeping the temperature for 3 hours;
and (3) carrying out film coating treatment (material chromium, thickness is less than 5nm) on the sample after the hot corrosion so as to enhance the conductivity of the ceramic sample and avoid the generation of a charge phenomenon during the observation of a scanning electron microscope.
And (3) placing the coated sample on a scanning electron microscope sample stage, placing the sample in a scanning electron microscope sample cavity, and carrying out imaging observation, wherein a shot picture is shown in figure 1, the contrast between a crystal boundary and crystal grains is obvious, small crystal grains are not peeled off, and the size distribution of the crystal grains is within the range of 100 plus 500 nm.
Example 2: scanning electron microscope image of hot corrosion section for preparing alumina ceramic
Preparing a ceramic biscuit with a relative density of 53% by using commercial alumina powder as a raw material and adopting a gel-casting method;
sintering the alumina ceramic biscuit for 3 hours at 1400 ℃ to obtain alumina ceramic with the relative density of 85 percent, breaking the sintered ceramic sample, and taking a fresh and clean section as a sample;
placing the sample in a muffle furnace for hot corrosion, wherein the corrosion temperature is 1000 ℃, and the heat preservation time is 3 hours;
and (3) carrying out film coating treatment (material chromium, thickness is less than 5nm) on the sample after the hot corrosion so as to enhance the conductivity of the ceramic sample and avoid the generation of a charge phenomenon during the observation of a scanning electron microscope.
And (3) placing the coated sample on a sample stage of a scanning electron microscope, placing the sample stage into a sample cavity of the scanning electron microscope, and carrying out imaging observation, wherein a shot picture is shown in figure 3, the contrast between crystal grains and a crystal boundary is obvious, pores are not damaged, small crystal grains are not peeled off, and the imaging is clear.
Example 3: scanning electron microscope image of acid corrosion section for preparing alumina ceramic
Preparing a ceramic biscuit with a relative density of 56% by using commercial alumina powder as a raw material and adopting a gel-casting method;
sintering the alumina ceramic biscuit for 6 hours at 1550 ℃ to obtain alumina ceramic with the relative density of 95 percent, breaking a sintered ceramic sample, and taking a fresh and clean section as a sample; the microstructure of the fresh section of the ceramic is shown in FIG. 5, and it can be seen that there is no contrast between the crystal grains and the grain boundaries in some regions, and only the grain boundaries in some regions are clear, and the ceramic sample is fractured in a partial transgranular fracture mode;
placing the sample in phosphoric acid (the concentration is 15mol/L) for corrosion, wherein the corrosion temperature is 300 ℃, and the heat preservation time is 30 minutes;
and (3) carrying out film coating treatment (the material is gold, and the thickness is less than 10nm) on the sample subjected to acid corrosion so as to enhance the conductivity of the ceramic sample and avoid the generation of a charge phenomenon during the observation of a scanning electron microscope.
And (3) placing the coated sample on a sample stage of a scanning electron microscope, placing the sample stage into a sample cavity of the scanning electron microscope, and carrying out imaging observation, wherein a shot picture is shown in fig. 4, the contrast between crystal grains and a crystal boundary is obvious, air holes are not damaged, small crystal grains are not peeled off, imaging is clear, and the size of the crystal grains is distributed in the range of 1-3 microns.
Example 4: scanning electron microscope image of hot corrosion section for preparing zirconia ceramic
Preparing a zirconia ceramic biscuit by using commercial zirconia powder as a raw material and adopting a cold isostatic pressing method;
presintering the zirconia ceramic biscuit for 3 hours in 1400 ℃ air atmosphere, sintering the biscuit for 3 hours in 1260 ℃ under 200MPa hot isostatic pressing to obtain zirconia ceramic with the relative density of 99.99 percent, breaking the sintered ceramic sample, and taking a fresh and clean section as a sample;
placing the sample in a muffle furnace for hot corrosion, wherein the corrosion temperature is 1000 ℃, and the heat preservation time is 3 hours;
and (3) carrying out film coating treatment (material chromium, thickness is less than 5nm) on the sample after the hot corrosion so as to enhance the conductivity of the ceramic sample and avoid the generation of a charge phenomenon during the observation of a scanning electron microscope.
And (3) placing the coated sample on a sample table of a scanning electron microscope, placing the sample table into a sample cavity of the scanning electron microscope, and carrying out imaging observation, wherein a shot picture is shown in fig. 6, the contrast between crystal grains and a crystal boundary is obvious, small crystal grains are not peeled off, the imaging is clear, and the size of the crystal grains is within the range of 30nm-300 nm.
Claims (6)
1. A sample preparation method for observing the microstructure in the ceramic by a scanning electron microscope is characterized in that a ceramic sample with submicron crystal grains is broken to obtain a fresh section, and then the fresh section is subjected to hot corrosion to obtain a ceramic material to be observed; the ceramic sample with the submicron-scale grains has a fracture mode of complete transgranular fracture or partial transgranular fracture, and the average grain size of the ceramic sample with the submicron-scale grains is less than 5 mu m;
the components of the ceramic sample comprise an oxide ceramic or a non-oxide ceramic; the oxide ceramic is magnesia-alumina spinel, zirconia or alumina, and the non-oxide ceramic is aluminum nitride, silicon carbide or boron nitride;
the temperature of the hot corrosion is 100-500 ℃ lower than the sintering temperature of the ceramic sample, and the time of the hot corrosion is 0.5-10 hours.
2. A method as claimed in claim 1, wherein the ceramic sample of submicron grains has an average grain size of less than 1 μm.
3. A sample preparation method as claimed in claim 1, wherein the ceramic sample is a dense ceramic or a porous ceramic.
4. A method as claimed in claim 3, in which the relative density of the non-porous skeletal region of the porous ceramic is greater than 65%.
5. A sample preparation method according to any one of claims 1 to 4, characterized in that the surface of the obtained ceramic material to be observed is subjected to a coating treatment; the film is made of gold, chromium or carbon, and the thickness of the film is less than or equal to 10 nm.
6. A ceramic material to be observed prepared according to the sampling method of any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010573950.9A CN111795984B (en) | 2020-06-22 | 2020-06-22 | Sample preparation method for observing microstructure inside ceramic by scanning electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010573950.9A CN111795984B (en) | 2020-06-22 | 2020-06-22 | Sample preparation method for observing microstructure inside ceramic by scanning electron microscope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111795984A CN111795984A (en) | 2020-10-20 |
| CN111795984B true CN111795984B (en) | 2022-05-10 |
Family
ID=72803661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010573950.9A Active CN111795984B (en) | 2020-06-22 | 2020-06-22 | Sample preparation method for observing microstructure inside ceramic by scanning electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111795984B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116660303B (en) * | 2023-07-31 | 2023-10-31 | 广东微容电子科技有限公司 | Analysis method of ceramic grains of multilayer ceramic capacitor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090074961A1 (en) * | 2007-09-19 | 2009-03-19 | Siemens Power Generation, Inc. | Engine portions with functional ceramic coatings and methods of making same |
| CN103319212A (en) * | 2013-07-12 | 2013-09-25 | 苏州微陶重金属过滤科技有限公司 | Preparation method of filtering material having arsenic and heavy metal adsorbing and fixing functions |
| CN103316544A (en) * | 2013-07-12 | 2013-09-25 | 苏州微陶重金属过滤科技有限公司 | Wastewater treatment filtering material, and preparation method and use thereof |
| CN109037759A (en) * | 2017-06-09 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | Prepare the sintering method of fine and close carbuncle type lithium ion solid electrolyte |
| CN110567998A (en) * | 2019-09-09 | 2019-12-13 | 中国科学院上海硅酸盐研究所 | Sample preparation method for rapidly obtaining silicon carbide ceramic crystal grain information and analysis and determination method thereof |
-
2020
- 2020-06-22 CN CN202010573950.9A patent/CN111795984B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090074961A1 (en) * | 2007-09-19 | 2009-03-19 | Siemens Power Generation, Inc. | Engine portions with functional ceramic coatings and methods of making same |
| CN103319212A (en) * | 2013-07-12 | 2013-09-25 | 苏州微陶重金属过滤科技有限公司 | Preparation method of filtering material having arsenic and heavy metal adsorbing and fixing functions |
| CN103316544A (en) * | 2013-07-12 | 2013-09-25 | 苏州微陶重金属过滤科技有限公司 | Wastewater treatment filtering material, and preparation method and use thereof |
| CN109037759A (en) * | 2017-06-09 | 2018-12-18 | 中国科学院上海硅酸盐研究所 | Prepare the sintering method of fine and close carbuncle type lithium ion solid electrolyte |
| CN110567998A (en) * | 2019-09-09 | 2019-12-13 | 中国科学院上海硅酸盐研究所 | Sample preparation method for rapidly obtaining silicon carbide ceramic crystal grain information and analysis and determination method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111795984A (en) | 2020-10-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5367080B2 (en) | Large ceramic rolling element | |
| JP5159310B2 (en) | Corrosion-resistant member and processing apparatus using the same | |
| Täffner et al. | Preparation and microstructural analysis of high-performance ceramics | |
| CN111795984B (en) | Sample preparation method for observing microstructure inside ceramic by scanning electron microscope | |
| CN110372386B (en) | Method for preparing compact tantalum carbide ceramic through low-temperature liquid-phase hot-pressing sintering | |
| WO2019235593A1 (en) | Plate-like silicon nitride sintered body and production method thereof | |
| CN110105057A (en) | Ceramic arm and preparation method thereof, vacuum suction machinery hand and wafer conveying device | |
| CN109336643A (en) | A kind of preparation method and composite material of silicon carbide ceramics surface laser cladding glass film layers | |
| CN111041448B (en) | Method for preparing diamond coating on surface of cobalt-containing hard alloy and tool and die with diamond coating | |
| WO2019235594A1 (en) | Plate-like silicon nitride sintered body and production method thereof | |
| Uematsu et al. | Effect of processing conditions on the characteristics of pores in hot isostatically pressed alumina | |
| US5472919A (en) | β-silicon nitride sintered body | |
| CN113462947A (en) | WC-based hard alloy and application thereof | |
| Sung et al. | Strength Improvement of Yttria‐Partially‐Stabilized Zirconia by Flaw Elimination | |
| JP4518020B2 (en) | A silicon nitride sintered body and a circuit board using the same. | |
| CN114605156B (en) | TiB 2 Composite ceramic material for base armor | |
| JP3775335B2 (en) | Silicon nitride sintered body, method for producing silicon nitride sintered body, and circuit board using the same | |
| CN114657524B (en) | Method for preparing gradient Nb-Si-based alloy film by adopting multi-target codeposition magnetron sputtering high-flux technology | |
| CN114195515B (en) | Oxide particle optimized nickel tantalate ceramic material and application thereof | |
| JP4546609B2 (en) | Ceramic heat treatment material with excellent thermal shock resistance | |
| Cengiz et al. | Characterization of coating formed on pure zirconium by MAO in yttrium acetate tetrahydrate containing electrolyte | |
| CN113728124A (en) | Member for plasma processing apparatus and plasma processing apparatus | |
| CN111058018A (en) | Preparation method of oxidation-resistant coating on surface of TD3 alloy | |
| CN110396603B (en) | Remelting method of iron-aluminum alloy | |
| JP2001172085A (en) | Silicon nitride sintered compact, production process therefor, and silicon nitride abrasion-resistant material using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |