CN111627827A - A method for judging the polar plane of single crystal by the difference of wettability - Google Patents
A method for judging the polar plane of single crystal by the difference of wettability Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000000758 substrate Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 20
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 20
- 238000005259 measurement Methods 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 229910002601 GaN Inorganic materials 0.000 claims description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 abstract description 3
- 238000001764 infiltration Methods 0.000 abstract description 3
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- 229910052799 carbon Inorganic materials 0.000 description 10
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- 239000010703 silicon Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 6
- 238000009736 wetting Methods 0.000 description 6
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
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- 125000004429 atom Chemical group 0.000 description 2
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- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
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Abstract
本发明涉及一种利用浸润鉴定单晶极性面的方法，包括：将需要判断的单晶材料制备成衬底，选定合适的液体作为判断的工具；在所述衬底的一个极性面上滴上所述液体，测量得到接触角α；在所述衬底的另一极性面上滴上所述液体，测量得到接触角β；根据两个接触角的大小，从而确定出两个极性面。本申请提供的方法一种能够快速有效、简单方便地解决目前鉴定单晶极性面大多比较费时费力甚至引起污染的问题。
The invention relates to a method for identifying the polar surface of a single crystal by infiltration, comprising: preparing a single crystal material to be judged into a substrate, selecting a suitable liquid as a tool for judgment; Drop the liquid on it, and measure the contact angle α; drop the liquid on the other polar surface of the substrate, and measure the contact angle β; according to the size of the two contact angles, determine the two Polar face. The method provided by the present application can quickly, effectively, simply and conveniently solve the problem that the identification of the polar surface of a single crystal is time-consuming and laborious, and even causes pollution.
Description
Technical Field
The present invention generally relates to the field of polar surface determination, and more particularly, to a method for determining a polar surface of a single crystal by using wettability differences.
Background
In production and life, single crystal materials such as third generation semiconductors represented by silicon carbide, zinc oxide and gallium nitride have wide application prospects in novel electronic devices, and the single crystals are paid more and more attention due to excellent performances of the single crystals. Single crystal samples also play an important role in scientific research, for example epitaxial growth requires a high quality single crystal as a substrate, the quality of which directly determines the purity of the grown material. With the above materials composed of two elements, the properties of the surface thereof are greatly different due to the difference in the polar planes. For example, silicon carbide, has two polar surfaces due to the difference in electronegativity between the carbon atoms and the silicon atoms that make up the silicon carbide: the carbon polar surface formed by carbon atoms and the silicon polar surface formed by silicon atoms have obvious difference in physical properties and chemical properties. In the use process of the single crystal, a reasonable polar surface needs to be correctly selected according to different application scenes, so that how to distinguish different polar surfaces is very important.
Most of the existing commonly used methods for identifying the polar surfaces of the single crystal are time-consuming, labor-consuming and even cause pollution, for example, for the single crystal of zinc oxide, one identification method is to use an acid solution to corrode the surface and distinguish different polar surfaces according to the difference of corrosion speeds. Such an identification method has great inconvenience in operation, such as corrosion using an acidic solution, discharge and treatment of acid solution, and environmental impact; at the same time, the process of identification damages the material, causing additional material waste. Therefore, the above method is not suitable for identifying the polar face quickly and efficiently. Other methods, while still under development, have several problems that need to be solved. Therefore, it is necessary to provide a method for rapidly, effectively, simply and conveniently identifying the polar face of a single crystal sample to solve the above problems.
Disclosure of Invention
The application aims to provide a method for identifying the polar surface of the single crystal, which is rapid, effective, simple and convenient, and solves the problems of time and labor waste and even pollution. To achieve the above object, the present application proposes a method for identifying a polar face of a single crystal by infiltration, comprising: preparing a substrate from a single crystal material to be judged, and selecting a proper liquid as a judging tool; dripping the liquid on one polar surface of the substrate, and measuring to obtain a contact angle alpha; dripping the liquid on the other polar surface of the substrate, and measuring to obtain a contact angle beta; according to the sizes of the two contact angles, two polar surfaces are determined.
In one example, the two contact angle values include: searching a contact angle of any polar surface of the single crystal material in a database; comparing said contact angle α and said contact angle β, respectively, to known contact angles of said either polar face; the polar surface on which the contact angle with smaller difference is located is the polar surface.
In one example, the two contact angle values include: searching the size relation of the contact angles of the two polar surfaces of the single crystal material in a database; comparing the magnitude of the contact angle alpha and the contact angle beta; and corresponding the comparison result to the magnitude relation to obtain the polarities respectively corresponding to the contact angle alpha and the contact angle beta.
In one example, the single crystal material is silicon carbide, zinc oxide, or gallium nitride.
In one example, the liquid is dropped to the substrate in the form of droplets.
In one example, the liquid is water.
In one example, the measurement is a plurality of measurements.
In an example, the contact angle α and/or the contact angle β is an average of the plurality of measurements.
Compared with the prior art, the method provided by the embodiment of the application has the advantages of no limitation of crystal size, no damage to materials, convenience, rapidness, low time cost and the like, can be widely applied to field production, meets the requirement of large-batch detection, and more importantly, obviously reduces the detection cost.
Drawings
The above and other objects, features and advantages of the present application will become more apparent by describing in more detail embodiments of the present application with reference to the attached drawings. The accompanying drawings are included to provide a further understanding of the embodiments of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the principles of the application. In the drawings, like reference numbers generally represent like parts or steps.
FIG. 1 is a flow chart of a method of operation of an embodiment of the present application.
FIG. 2 is an example of 6H-type silicon carbide, showing the difference in the morphology of water droplets on the carbon polar surface and the silicon polar surface.
FIG. 3 shows the contact angles on the different polarity planes of the silicon carbide samples having the same type 6H and different conductivity characteristics.
FIG. 4 is a graph showing contact angles on different polar surfaces of samples of silicon carbide having the same type 4H but different conductivity characteristics.
Fig. 5 is a contact angle on both polar faces of a zinc oxide single crystal.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely exemplary of some of the present application and that the present application is not limited to these exemplary embodiments described herein.
The existing theoretical results show that the wetting behavior of a water drop on the surface of a substrate is easily influenced by the properties of atomic scale and is expressed in the form of contact angle, and the contact angle can be easily measured by an instrument and even can be observed by naked eyes in a certain obvious phenomenon. Theoretically, the main effects on wetting are van der waals and electrostatic effects. The former is short-range action, with a very small range of action, approximately 1 nanometer. The latter, although a long-range effect, still shows a large difference in its effect on polar liquids (e.g. water) in view of the positive and negative electrical properties. The reason for this is that water is a very polar liquid, and water molecules have a V-shaped structure. On the polar surfaces generated by different electric properties, the arrangement state of the part of water molecules closest to the polar surfaces is completely different. For example, on a polar face that is electropositive near the surface, the oxygen atoms in the water molecule are closer to the surface; on the polar face where the electronegativity is close to the surface, the hydrogen atoms in the water molecules are closer to the surface. Scientific studies have confirmed that which atoms are closer to the surface directly determines the wetting behavior of the entire water droplet. Therefore, the difference of the polar faces can generate different wetting behaviors, and has a definite theoretical basis.
The contact angle magnitude relation of different polar surfaces can be obtained by the following two ways: first, by computer simulation or search of relevant literature, such as silicon carbide, the applicant of the present application found in previously published articles that the contact angle of a water drop on the polar face of silicon is smaller than that on the polar face of carbon; second, the contact angles of water drops on two polar surfaces are measured and the relationship between the two contact angles is compared when the oxygen polar surface and the zinc polar surface are known, and the relationship between the contact angles is directly used for discrimination in the subsequent identification, thereby facilitating the subsequent identification.
Based on the above theoretical analysis, the present application provides a method for identifying the polar surface of a single crystal material by using the wetting difference. The single crystal has many kinds, and different kinds generate different configurations due to growth conditions such as doping, temperature and the like. Different configurations of the same material generate different polar surfaces due to different atoms, for example, silicon carbide has a carbon polar surface and a silicon polar surface, and the carbon polar surface and the silicon polar surface have different properties in a production process and need to be distinguished and selected according to specific application scenarios. The problem to be solved by the present application is to identify differently polar faces of a single crystal.
Specifically, the implementation method of the present application is described in detail in conjunction with the flowchart of fig. 1.
S100: preparing a substrate from a single crystal material to be subjected to polarity identification, and selecting a proper liquid as a tool for judgment. The planar size of the substrate requires that a droplet with a diameter of 2 mm or more can be placed; the thickness of the substrate has no special requirement, and the thickness of the common crystal at present can be all; the wetting is measured independently of the shape of the substrate, and therefore there are no special requirements on the shape of the substrate. For the treatment of the substrate, the substrate can be cleaned by adopting methods such as soaking, ultrasonic, infrared, drying and the like, so that the surface of the substrate is free from the pollution of impurities; simultaneously, processing two polar surfaces of the substrate to be consistent or similar in polishing degree; the measurement operation is performed in a relatively clean environment to avoid contamination of the surface of the substrate by dust and the like in the atmosphere; contact with the substrate surface is avoided during measurement to maintain the substrate clean. In theory, the conditions should be consistent except for the different polarity planes of the materials.
S200: a droplet is dropped on one polar side of the substrate and the contact angle α is measured. The liquid drop placement process is as gentle and stable as possible, and large jitter is avoided when the liquid drop falls on the surface of the substrate; the measurement should be performed immediately after the drop is placed (e.g., half a minute or less) to avoid the drop evaporating causing inaccurate measurement results; the volume of the drop is not limited by the strict size (for general materials, 0.2 microliter to 2 microliter, other materials can be adjusted as appropriate), but the size of the drop on the different polar surfaces is ensured to be consistent.
Specifically, referring to fig. 2, before measurement, a material to be subjected to polarity surface identification is selected as a substrate, so that the substrate material is ensured to be clean, and the substrate surface is ensured to be suspended and horizontally placed as much as possible without contacting other pollutants on the sample stage, so as to avoid affecting the accuracy of the measured value.
During measurement, firstly, liquid drops are slowly placed on the surface of a substrate material to be identified, and large jitter is prevented from occurring in the placing process; the droplet is positioned as far as possible in the middle part of the substrate. The difference of the contact angles is large in the single crystal material with the polarity having large influence on the infiltration, and the polar surface of the material can be very intuitively judged by measurement; if the measurement results show that the contact angle of a certain droplet (such as a water droplet) is not very different, a liquid with a larger surface tension can be selected or the droplet can be treated, for example, by adding a salt (such as sodium chloride) to the droplet to increase the surface tension.
Secondly, after a side view of the water drop is shot, firstly, circular or elliptical fitting is carried out on the outer contour of the side view by using a least square method to obtain the shape of the outer contour; meanwhile, determining the boundary between the substrate and the water drop and taking the boundary as a datum line; and then, calculating the included angle between the tangent line of the circle or the ellipse obtained above at the reference line and the reference line, wherein the included angle is the contact angle and is a required numerical value. The contact angle value of the liquid drop on the surface of the polar material can be determined by adopting a method of measuring for multiple times, repeating the above operations to obtain several values, and taking the average value of the values as a final result. It should be understood that in order to ensure the accuracy of the measurement, it is endeavored to ensure that the surface roughness of the differently polar surfaces being measured is substantially the same.
S300: and (4) dropping a liquid drop on the other polar surface of the substrate, and measuring to obtain a contact angle beta, wherein the specific operation steps and requirements are the same as those of S100 and S200.
S400: and comparing the sizes of the two contact angles, and determining two polar surfaces according to the information of the database.
Specifically, a database is established by performing data acquisition records in the early stage. For example, for each type of material with known polar surfaces, the contact angles of a liquid drop on two polar surfaces are measured respectively, the relationship between the two contact angles is compared, and the measurement results are counted in a database, for example, according to the following formula "material a: polar plane a1, contact angle α 1; polar plane a2, contact angle α 2; α 1 < α 2 … … "are registered. It will be appreciated that the database may also be formed by obtaining contact angle data for polar surfaces by other means such as literature or classical molecular dynamics calculations.
In the subsequent identification, for different materials, the contact angles measured in the steps S100-S400 are compared with each other, and the data of the corresponding materials are matched, so that the polar surfaces corresponding to the different contact angles can be directly obtained.
In particular, there are various ways of operating the polar surface based on the measured contact angle.
In one example, the contact angle Δ of any polar face of the single crystal material can be first looked up in a database; then, the contact angle alpha and the contact angle beta measured in the step are respectively compared with the known contact angle of any polar surface to obtain comparative values | delta-alpha | and | delta-beta |; if | Δ - α | is smaller than | Δ - β |, the polar surface on which the contact angle α is located is the polar surface corresponding to the contact angle Δ, and if | Δ - β | is smaller than | Δ - α |, the polar surface on which the contact angle β is located is the polar surface corresponding to the contact angle Δ.
In another example, the magnitude relationship of the contact angles a and B of the two polar surfaces of the single crystal material can be first searched in the database, for example, a > B; the contact angle α and the contact angle β are then compared in magnitude, e.g., α > β; the contact angle alpha corresponds to the contact angle A, the contact angles beta respectively correspond to the contact angles B, the polar surface where the corresponding contact angle alpha is located is the polar surface corresponding to the contact angle A, and the polar surface where the contact angle beta is located is the polar surface corresponding to the contact angle B.
Based on the above method, the following example can be implemented.
Example one:
step 1: selecting a material needing polarity surface identification as a substrate to ensure the cleanness of the substrate material;
step 2: slowly placing water drops on the surface of the substrate material to be identified, and ensuring that no large jitter occurs in the placing process;
and step 3: measuring the contact angle value of the water drop on the polar surface;
and 4, step 4: repeating the steps 2 and 3 on the other polar surface of the material, and measuring the contact angle value of the water drop on the polar surface.
And 5: and determining the polar surface according to the existing data and the numerical value relationship of the two contact angles.
Example two:
step 1: selecting a material needing polarity surface identification as a substrate to ensure the cleanness of the substrate material;
step 2: slowly placing liquid drops (the components are nonaqueous but polar liquid) on the surface of the substrate material to be identified, and ensuring that large jitter does not occur in the placing process;
and step 3: measuring the contact angle value of the liquid drop on the polar surface;
and 4, step 4: repeating the steps 2 and 3 on the other polar surface of the material, and measuring the contact angle value of the liquid drop on the polar surface.
And 5: and determining the polar surface according to the existing data and the numerical value relationship of the two contact angles.
It should be understood that in some particular cases, other liquids may be used in addition to water droplets as identification droplets.
Example three:
step 1: placing a water drop or other liquid drops on the surface of a material needing polar surface identification, measuring the contact angle of the liquid drop, and recording the value 1 of the contact angle;
step 2: when the contact angle value of a certain polar surface is known, the contact angle value 1 is directly compared with the value, and when the difference between the two values is 4 degrees or more, the state of the polar surface can be directly judged. Wherein, the contact angle value in the step needs to be characterized in advance, and a reasonable contact angle value and an error range are obtained. Specifically, the data acquisition record can be performed at an earlier stage to establish a database. For example, for each type of material with known polar surfaces, the contact angles of a liquid drop on two polar surfaces are measured respectively, the relationship between the two contact angles is compared, and the measurement results are counted in a database, for example, according to the following formula "material a: polar plane a1, contact angle α 1; polar plane a2, contact angle α 2; α 1 < α 2 … … "are registered. It will be appreciated that the database may also be formed by obtaining contact angle data for polar surfaces by other means such as literature or classical molecular dynamics calculations.
To demonstrate the feasibility of the above method, the inventors of the present application further described the theoretical basis of the present application in detail by taking silicon carbide in both 6H and 4H configurations after the same polishing treatment as an example.
Fig. 2 is an example in which a 6H-type silicon carbide material is used as a substrate and water is used as a liquid. It can be obviously seen that the difference between the shapes of water drops on the carbon polar surface and the silicon polar surface of the 6H-type silicon carbide is very obvious, and the difference is reflected in the measurement of the contact angle, and the corresponding contact angles are 34 degrees and 11 degrees respectively. According to the existing theory, the difference of the shapes of the water drops shows the property difference of two polar surfaces, namely a carbon polar surface with a large contact angle and a silicon polar surface with a small contact angle.
Fig. 3 shows contact angles on different polar surfaces of the silicon carbide sample having different conductivity characteristics, which are the same type 6H, and it can be seen that the contact angles on the carbon polar surfaces are all larger than those on the silicon polar surfaces, which indicates that the polar surfaces are not affected by the conductivity of silicon carbide by using the contact angles.
FIG. 4 is a graph showing the contact angles on the different polar surfaces of the silicon carbide samples having the same 4H type and different conductive characteristics, wherein the contact angles on the carbon polar surfaces are all larger than the contact angles on the silicon polar surfaces. In conjunction with fig. 3, the use of contact angles to identify polar planes is illustrated as unaffected by the crystalline form of silicon carbide. Also, the results again demonstrate that the use of contact angles to identify polar planes is not affected by the conductivity of silicon carbide.
It can be seen that for silicon carbide with both 6H and 4H configurations, the contact angle of the carbon polar face is larger than that of the silicon polar face, and the difference of the contact angles can even reach more than 20 degrees. Moreover, this difference is independent of the conductivity type of the silicon carbide. Therefore, the method for judging the polar surface by using the contact angle has greater universality and can be used for identifying different polar surfaces.
Fig. 5 is an example of a substrate made of a zinc oxide single crystal material. As can be seen from the figure, the contact angle on the zinc polar surface of the zinc oxide single crystal is larger than that on the oxygen polar surface, and the method shown in the application is further proved to be suitable for the identification of the zinc oxide single crystal polar surface.
It will be appreciated that although the above embodiments are exemplified by the contact angle of water with a polar surface, other liquids may be adaptively selected for operation as desired.
The feasibility of judging the polar plane of a single crystal material by contact angle was further demonstrated in conjunction with the above-described graphical illustration. In combination with the description of the embodiment, it can be seen that the method for identifying different polar surfaces by using the difference of wettability (i.e. the size of the contact angle) provided by the application has the advantages of time and labor saving, rapidness, high efficiency, low cost, no damage to single crystal materials, no limitation of single crystal size and the like compared with other identification methods, can meet the requirements of enterprise production, laboratories and other occasions on polar surface identification, is suitable for large-scale identification requirements, and can reduce the detection cost.
The above-mentioned embodiments, objects, technical solutions and advantages of the present application are described in further detail, it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present application, and are not intended to limit the scope of the present application, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present application should be included in the scope of the present application.
Claims (8)
1. A method for judging a polar surface of a single crystal by using wettability differences comprises the following steps:
preparing a substrate from a single crystal material to be judged, and selecting a proper liquid as a judging tool;
dripping the liquid on one polar surface of the substrate, and measuring to obtain a contact angle alpha;
dripping the liquid on the other polar surface of the substrate, and measuring to obtain a contact angle beta;
according to the sizes of the two contact angles, two polar surfaces are determined.
2. The method of claim 1, wherein the two contact angle values comprise:
searching a contact angle of any polar surface of the single crystal material in a database;
comparing said contact angle α and said contact angle β, respectively, to known contact angles of said either polar face;
the polar surface on which the contact angle with smaller difference is located is the polar surface.
3. The method of claim 1, wherein the two contact angle values comprise:
searching the size relation of the contact angles of the two polar surfaces of the single crystal material in a database;
comparing the magnitude of the contact angle alpha and the contact angle beta;
and corresponding the comparison result to the magnitude relation to obtain the polarities respectively corresponding to the contact angle alpha and the contact angle beta.
4. The method of claim 1, wherein the single crystal material is silicon carbide, zinc oxide, or gallium nitride.
5. The method of claim 1, wherein the liquid is dripped onto the substrate in the form of droplets.
6. The method of claim 1, wherein the liquid is water.
7. The method of claim 1, wherein the measurement is a plurality of measurements.
8. The method of claim 7, wherein the contact angle a and/or the contact angle β is an average of the plurality of measurements.
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| CN116165339A (en) * | 2022-12-20 | 2023-05-26 | 中国科学院物理研究所 | Method for determining silicon and carbon surfaces of silicon carbide wafers |
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| W.W.ZHONG等: "Wetting behavior of water on silicon carbide polar surfaces", 《PHYS. CHEM. CHEM. PHYS.》 * |
| WANGYANG ZHANG等: "Optically Induced Rapid Wetting Transition on Zn-Polar and O-Polar Zinc Oxide", 《LANGMUIR》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116165339A (en) * | 2022-12-20 | 2023-05-26 | 中国科学院物理研究所 | Method for determining silicon and carbon surfaces of silicon carbide wafers |
| CN116165339B (en) * | 2022-12-20 | 2025-03-21 | 中国科学院物理研究所 | Method for determining the silicon side and the carbon side of a silicon carbide wafer |
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