Multi-layer material, abrasive material used by same and application of multi-layer material

Abstract

The embodiment of the invention provides a multi-layer material, an abrasive material used by the multi-layer material and application, the abrasive material is a foamed sheet of a polyester elastomer, and the loss factor of the abrasive material at any temperature within the range of 25-85 DEG C is smaller than 0.1. When the polyester elastomer is used for the grinding material, the multilayer material adopting the grinding material can be ensured to have a very good elastic recovery rate, and the planarization rate of a base material is stable.

Description

Technical Field

[0001] The present application relates to the technical field of multilayer materials, and in particular to a multilayer material and a grinding material and application thereof. Background Art

[0002] Multilayer materials are an important auxiliary material required for the flattening of substrate surfaces. They can store and transport the working fluid for flattening and work together with the working fluid to achieve flattening of the substrate. Multilayer materials usually include a stacked base layer, an adhesive layer, and a porous grinding layer. The grinding layer is in contact with the substrate to be treated and is the core functional layer that affects the flattening result.

[0003] In the currently commercially available or reported multilayer materials, the grinding layer is usually a polyurethane elastomer with a porous structure, but the elastic modulus of the existing polyurethane elastomer varies greatly within the working range of the multilayer material, resulting in an unstable flattening rate of the substrate, and even blocking of the pores and premature end of life. With the development of flattening technology and the demand for flattening of diversified substrates, new elastomer materials should be used in multilayer materials, and can ensure the stability of the flattening rate of the multilayer material to the substrate. Summary of the invention

[0004] In view of this, an embodiment of the present application provides a polishing layer material that can be used for multi-layer materials to solve the problem of unstable planarization rate of the existing multi-layer materials on the substrate.

[0005] A first aspect of an embodiment of the present application provides an abrasive material for surface treatment of a substrate, wherein the abrasive material is a foamed sheet of a polyester elastomer, and the loss factor of the abrasive material at any temperature within the range of 25-85°C is less than 0.1.

[0006] The present application adopts a foamed sheet of polyester elastomer as a grinding material for surface treatment of a substrate, and controls the loss factor of the grinding material within the temperature range of the flattened substrate to be less than 0.1, indicating that it has less endogenous heat and a high elastic recovery rate, which can ensure that the flattening rate of the multilayer material using the grinding material for the substrate is stable and has a long service life.

[0007] In the embodiment of the present application, the elastic recovery rate of the abrasive material is above 90%, which indicates that the external force mainly causes elastic deformation, less internal heat is generated, and the service life of the abrasive material is long.

[0008] In the embodiment of the present application, the elastic recovery rate of the grinding material is above 90% after being subjected to 50,000 compression fatigue tests with a deformation amount of 20%, which can better reflect that the compression resilience of the polyester elastomer foam sheet provided in the present application is better.

[0009] In the embodiment of the present application, the relative standard deviation of the thickness of the same foamed sheet does not exceed 10%, which reflects that the thickness of the foamed sheet of polyester elastomer at different positions is highly uniform, thereby ensuring that the grinding degree of different positions of the substrate is highly consistent.

[0010] In the embodiment of the present application, the polyester elastomer includes a polyester hard segment and a polyether soft segment, wherein the polyester hard segment is selected from one or more of polyethylene terephthalate, polybutylene terephthalate, and polypropylene terephthalate; the polyether soft segment includes one or more of a polytetrahydrofuran diol segment, a polyoxypropylene diol segment, and a polyoxyethylene diol segment.

[0011] In the embodiment of the present application, the grinding material is obtained by subjecting the formed sheet containing the polyester elastomer to vacuum heat treatment and then to supercritical foaming. The formed sheet of the polyester elastomer is first subjected to vacuum heat treatment before supercritical foaming, so that its stress can be released, and the structural defects can be improved or eliminated, so that the thickness uniformity of the obtained foamed sheet is higher and the compression resilience becomes better.

[0012] A second aspect of an embodiment of the present application provides a multilayer material, which includes a base layer, an adhesive layer and a grinding layer stacked in sequence, wherein the grinding layer includes the grinding material as described in the first aspect of the embodiment of the present application.

[0013] The multilayer material for flat substrates introduces the above-mentioned grinding layer material with good performance, which can ensure that the multilayer material has less internal heat generated under the action of external force, the grinding rate of the substrate is stable, the flattening effect of the substrate after different batches of processing is similar, and the service life of the multilayer material is long.

[0014] A third aspect of the embodiments of the present application provides a substrate surface treatment device, which includes the multilayer material described in the second aspect of the embodiments of the present application.

[0015] In some embodiments of the present application, the substrate surface treatment device includes a working platform and a grinding head suspended above the working platform, the surface of the working platform is provided with the multi-layer material, or the multi-layer material is installed on the grinding head.

[0016] By using a substrate surface treatment device with the multilayer material, the flattening rate of the substrate surface is stable and the flattening effect is good, scratches are not easily generated on the substrate surface, and the device has a long service life.

[0017] The present invention also provides a method for preparing an abrasive material, comprising the following steps:

[0018] forming a polyester elastomer into a sheet for foaming;

[0019] The foaming sheet is subjected to vacuum heat treatment and then supercritical foaming to obtain a grinding material; wherein the grinding material is a foaming sheet of a polyester elastomer, and the loss factor of the grinding material at any temperature within the range of 25-85°C is less than 0.1.

[0020] Before the polyester elastomer sheet to be foamed is subjected to supercritical foaming, a vacuum heat treatment is first performed, so that the original bubbles in the sheet can be squeezed out, the stress can be released, and various structural defects caused during the molding process can be improved or eliminated, thereby improving the thickness uniformity and pore size uniformity of the foamed sheet obtained by foaming, while ensuring that the compression resilience becomes better, so that the loss factor of the obtained grinding material at any temperature in the range of 25-85°C can be less than 0.1. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1A and Figure 1B Two schematic structural diagrams of the multilayer material 100 provided in the embodiments of the present application.

[0022] Figure 2 A schematic structural diagram of a substrate surface treatment device 200 provided in an embodiment of the present application.

[0023] Figure 3 The loss factor curves of the grinding layer samples of Examples 1-2 and Comparative Example 1 provided in the present application at different temperatures. DETAILED DESCRIPTION

[0024] The technical solution of the present application will be described below in conjunction with the drawings in the embodiments of the present application.

[0025] Multilayer materials are important auxiliary materials that determine the surface treatment quality of the substrate to be treated (such as semiconductor substrates, glass, metal, ceramics, optical devices, etc.) in the surface flattening process. Please also refer to Figure 1A and Figure 1B The multilayer material 100 for substrate surface treatment provided in the embodiment of the present application includes a base layer 11, an adhesive layer 12 and a grinding layer 13 with a porous structure which are stacked in sequence.

[0026] Among them, the surface of the base layer 11 away from the grinding layer 13 is the adsorption surface of the multilayer material 100, which is used to ensure that the multilayer material 100 is attached to the substrate surface treatment device. The surface of the grinding layer 13 away from the base layer 11 is the working surface of the multilayer material 100, which is used to contact the surface to be processed of the substrate, so that the substrate obtains a flat surface under the mechanical action of the multilayer material 100 and the chemical action of the grinding working fluid. During the flattening process of the substrate, the multilayer material will undergo multiple compressions and rebounds. If the compression resilience of the grinding layer 13 is not good, its interior and surface are prone to deformation and collapse of the pore structure, resulting in an unstable flattening rate of the substrate. Therefore, when developing new grinding layer materials that can be used for the multilayer material 100, it is necessary to ensure that the flattening rate of the multilayer material to the substrate is stable.

[0027] An embodiment of the present application provides a material that can be used for the grinding layer 13 in the multilayer material 100. The grinding material is a foamed sheet of polyester elastomer. The loss factor of the grinding material at any temperature in the range of 25-85°C (denoted as Tanδ(25~85°C)) is less than 0.1.

[0028] Among them, 25°C is the common starting working temperature of multilayer materials, and 85°C is the common maximum working temperature of multilayer materials. The loss factor of the constituent materials of the grinding layer 13 controlled by the present application is less than 0.1 within the working temperature range of the multilayer material (25-85°C). This indicates that within the above temperature range, it mainly undergoes elastic deformation under the action of external force, with less endogenous heat, high elastic modulus, and low loss modulus E", so the Tanδ value (=E" / E') is low, and there will be no sudden change point of sudden increase / decrease in elastic modulus. After the external force is removed, the material can basically recover to the initial deformation, with good resilience and low probability of plastic deformation, and the probability of its pore structure being blocked / collapsed due to plastic deformation is also low, thereby ensuring that the grinding rate of the grinding material on the substrate is stable during its working process and improving its own service life.

[0029] In some embodiments of the present application, the loss factor of the above-mentioned grinding material at any temperature in the range of 25-85° C. is less than or equal to 0.08, less than or equal to 0.075, less than or equal to 0.06, less than or equal to 0.05, etc. In this case, the grinding layer generates less heat under stress during the operation of the multilayer material 100, has better compression resilience, and is more conducive to maintaining a stable planarization effect of the multilayer material 100.

[0030] The loss factor Tanδ of the grinding material at different temperatures can be obtained based on the dynamic mechanical analysis (DMA) test. Each Tanδ can be measured according to the standard ISO6721-4, with a test frequency of 1 Hz and a heating rate of 3°C / min.

[0031] In the embodiment of the present application, the elastic recovery rate of the above-mentioned grinding material is above 90%. The elastic recovery rate of the polyester elastomer foam sheet after being compressed is above 90%, indicating that the external force mainly causes its elastic deformation and less internal heat generation. After the grinding layer 13 completes the surface treatment of the substrate, it can basically recover to its original shape, thereby ensuring that the multilayer material 100 has good reusability. The above-mentioned elastic recovery rate can be measured according to the national standard GB / T 20671.2-2006.

[0032] In the embodiment of the present application, the above-mentioned abrasive material can still have an elastic recovery rate of more than 90% after being subjected to 50,000 compression fatigue tests with a deformation of 20%. This can better reflect that the foamed sheet of the polyester elastomer provided by the present application has particularly excellent compression resilience, which is conducive to the multilayer material 100 using the abrasive material to maintain a very close rebound level in the early and later stages of use.

[0033] In the embodiment of the present application, the grinding material is a foam sheet, and the thickness relative standard deviation of the same foam sheet does not exceed 10%, and can further be less than or equal to 6%, less than or equal to 5%, etc. The thickness relative standard deviation can be obtained by testing and calculating the thickness of the foam sheet at different positions. in, σ1 is the standard deviation of the thickness measured at multiple different locations of the foam sheet, Represents the average value of the thickness measured at multiple different locations of the foam sheet, D i represents the specific thickness value measured at each different position of the same foamed sheet, and n represents the number of different positions selected.

[0034] The lower RSD means that the thickness of the foamed sheet of polyester elastomer at different positions is highly uniform. When the multilayer material made of the polyester elastomer is ground on the surface of the substrate, the grinding degree of different positions of the substrate can be ensured to be consistent, and the grinding effect of substrates processed in different batches can be ensured to be similar. After the polyester elastomer is treated by the vacuum heat treatment-supercritical foaming process provided below in this application, the thickness of the foamed sheet obtained is more uniform and the cell size is more uniform.

[0035] In the embodiment of the present application, the grinding material is a foam sheet, and the ratio of the minimum thickness to the maximum thickness of the same foam sheet is above 90%, and can be above 95%, which reflects that the thickness of the foam sheet does not fluctuate much and has good uniformity.

[0036] In the present application, the above-mentioned grinding material is a foamed sheet with a porous structure. In the embodiment of the present application, the average pore size (i.e., average pore size) of the grinding material is 5μm-50μm. Suitable average pore size is conducive to the rapid delivery of grinding working fluid, ensuring that the multilayer material 100 processes the substrate at a faster speed, while reducing the surface defects of the substrate after treatment. In some embodiments, the average pore size of the grinding material is 10μm-40μm, for example, specifically 15μm, 20μm, 25μm, 30μm, 35μm or 39μm, etc. Among them, the average pore size can be measured from the scanning electron microscope (SEM) photo of the grinding material. Specifically, the surface of the grinding material can be magnified to 100 times for SEM observation, and the image is binarized using the image processing software Image J to confirm the number of bubbles, and the average bubble diameter is further calculated by the sum of the open area of ​​each bubble.

[0037] In the embodiment of the present application, the surface porosity of the grinding material is in the range of 20%-80%. In other words, the porosity of the surface of the grinding layer 13 away from the base layer 11 is controlled in the range of 20%-80%. This is conducive to the multilayer material 100 having a suitable processing rate and a good processing effect on the substrate to be processed. If the surface porosity of the grinding layer 13 is too low, its carrying capacity for the working fluid is insufficient, and the processing rate of the substrate will be discounted; if the surface porosity is too high, it is easy to cause the thrown waste to fill the surface pores, affecting the subsequent processing effect. Among them, the above-mentioned surface porosity can be obtained by obtaining a scanning electron microscope photograph of the working surface of the grinding layer 13 (the magnification can be 100 times) to obtain the ratio of the area occupied by the bubbles on it to the area of ​​the surface.

[0038] In the embodiment of the present application, the density of the above-mentioned grinding material is 0.3-1.0g / cm 3 The density in this range can reflect to some extent that the grinding layer 13 is light in weight and has a porous structure with a suitable porosity to transport the grinding working fluid, while at the same time not being too light in density to affect its mechanical properties. Specifically, the density of the grinding material can be 0.4 g / cm 3 , 0.5g / cm 3 , 0.6g / cm 3 , 0.7g / cm 3 , 0.71g / cm 3 , 0.72g / cm 3 , 0.75g / cm 3 , 0.8g / cm 3 , 0.85g / cm 3 wait.

[0039] In the embodiment of the present application, the Shore hardness of the above-mentioned grinding material is in the range of 15A-60D. The present application selects a polyester elastomer of suitable hardness for foaming, and the obtained foamed material has good resilience and suitable hardness, which increases its own wear resistance, ensures the flattening effect on the surface of the substrate, and is not easy to scratch the substrate. In some embodiments, the Shore hardness of the above-mentioned grinding material is 30D-50D, and can further be 31D-40D.

[0040] In the present application, the polyester elastomer is a linear block copolymer containing a polyester hard segment and a polyether soft segment, which has both the excellent elasticity of rubber and the easy processability of thermoplastics, and the hardness and softness are adjustable. Among them, the polyester elastomer can be prepared by transesterification and polycondensation of dimethyl terephthalate with a small molecule diol (such as ethylene glycol, propylene glycol, butanediol, etc.) and a polyether polyol. Among them, the polyester hard segment of the polyester elastomer has a repeating unit derived from the transesterification-polycondensation reaction product of dimethyl terephthalate and a small molecule diol, and the polyether soft segment has a repeating unit derived from the transesterification-polycondensation reaction product of dimethyl terephthalate and a polyether polyol.

[0041] In the embodiment of the present application, the polyester hard segment of the polyester elastomer may include one or more of polyethylene terephthalate (PET), polybutylene terephthalate (PBT), and polypropylene terephthalate (PTT), but is not limited thereto. The polyether soft segment of the polyester elastomer may include one or more of polytetramethylene ether glycol (PTMEG) segment, polyoxypropylene glycol (PPG) segment, and polyoxyethylene glycol (PEG) segment, but is not limited thereto.

[0042] In the embodiment of the present application, the grinding material is obtained by vacuum heat treatment of a shaped sheet containing a polyester elastomer and then supercritical foaming. The shaped sheet of the polyester elastomer is first subjected to vacuum heat treatment before supercritical foaming, which can release its stress and improve or eliminate its structural defects, so that the thickness uniformity of the obtained foamed sheet is higher and the compression resilience becomes better.

[0043] The present application also provides a method for preparing the above-mentioned grinding material. Specifically, the method for preparing the grinding material may include the following steps:

[0044] forming the polyester elastomer into a sheet to be foamed;

[0045] The sheet to be foamed is subjected to vacuum heat treatment and then supercritical foaming to obtain a grinding material; wherein the grinding material is a foamed sheet of polyester elastomer, and the loss factor of the grinding material at any temperature within the range of 25-85°C is less than 0.1.

[0046] Among them, before the foaming sheet is subjected to supercritical foaming, a vacuum heat treatment is first performed, which can squeeze out the original bubbles inside, release the stress, and improve or eliminate various structural defects caused during its molding process, thereby improving the thickness uniformity and pore size uniformity of the foamed sheet obtained by foaming, while ensuring that the compression resilience becomes better, and the loss factor at any temperature in the range of 25-85°C can be less than 0.1.

[0047] In the embodiment of the present application, the treatment temperature of the vacuum heat treatment is between T m -20℃ to T m ℃, the treatment time is 1-10 hours; among which, T m represents the melting point of the polyester elastomer.

[0048] Among them, the vacuum condition is conducive to the removal of bubbles in the foamed sheet; between T m -20℃ to T m The vacuum heat treatment temperature between 100°C and 200°C can cause the sheet to be foamed to undergo a proper degree of micro-melting without changing the overall structural configuration, so that various tissue defects therein are improved or eliminated, and the unevenness of the surface is improved. At the same time, after the vacuum condition is removed, it is not easy to introduce new bubbles. In addition, sufficient vacuum heat treatment time can ensure that the above-mentioned various improvement effects are fully presented. In some embodiments, the treatment temperature of the vacuum heat treatment is in the range of 120-150°C, for example, specifically 125, 130, 135, 140 or 145°C. Furthermore, the vacuum degree during the vacuum heat treatment is less than 0.08MPa.

[0049] In the embodiment of the present application, the molding method of molding the polyester elastomer material into the sheet to be foamed includes but is not limited to one or more of extrusion molding, hot pressing molding, injection molding, etc. Using a sheet-shaped molded product for foaming can ensure that the obtained foaming material is also a sheet, and the shapes of the two are highly corresponding, but the thickness, density, etc. of the two are different.

[0050] Supercritical foaming molding is a physical foaming molding technology, which uses supercritical fluid as a foaming agent and performs foaming at a certain foaming pressure and foaming temperature. "Supercritical fluid" refers to a special state in which a substance is in a temperature and pressure above its supercritical point. In this state, the fluid has both gas and liquid properties, such as its viscosity and diffusion coefficient are similar to those of a gas, and its density and solvation ability are similar to those of a liquid. In the embodiment of the present application, the supercritical fluid used can be selected from one or more of supercritical nitrogen (N2) and supercritical carbon dioxide (CO2).

[0051] Among them, the supercritical foaming process may include:

[0052] 1) placing the sheet to be foamed after vacuum heat treatment in a foaming cavity, and heating the foaming cavity to a preset foaming temperature;

[0053] 2) introducing a supercritical fluid into the foaming cavity, making the pressure in the foaming cavity reach a preset foaming pressure, and maintaining the preset foaming temperature and the preset foaming pressure for a period of time so that the supercritical fluid reaches a dissolution equilibrium in the sheet to be foamed;

[0054] 3) Relieving the pressure of the foaming cavity to foam the sheet to be foamed to obtain a foamed sheet.

[0055] In step 1), the preset temperature can be set according to the melting point of the supercritical fluid and the polyester elastomer used. The preset temperature should be higher than the critical temperature of the supercritical fluid and the glass transition temperature Tg of the polyester elastomer, so that the fluid is in a supercritical state and the sheet to be foamed has a suitable melt strength for foaming. Correspondingly, in step 2), when the supercritical fluid is introduced into the foaming cavity, the preset foaming pressure reached in the foaming cavity should be higher than the critical pressure of the supercritical fluid, so that the fluid is in a supercritical state, which is convenient for diffusion into the sheet to be foamed and achieves a higher solubility therein. In some embodiments, when the supercritical fluid is supercritical CO2 and / or N2, the preset foaming pressure can be in the range of 10-20 MPa, for example, 10, 12, 15 or 18 MPa, etc., and can further be 10-15 MPa; the preset foaming temperature can be in the range of 120-160°C, for example, 125, 130, 135, 140, 150, 155, 158°C, etc.

[0056] In step 2), the preset foaming temperature and the preset foaming pressure are maintained for a period of time (this holding time can be called "saturation time"), so that the supercritical fluid can fully diffuse into the sheet to be foamed and reach a dissolution equilibrium therein. After that, the pressure difference between the pressure inside the sheet to be foamed and the external environmental pressure can be caused by the pressure relief in step 3), resulting in the supercritical fluid dissolved in the sheet to be foamed being in a thermodynamically unstable state, and a large number of cell nuclei are generated in the sheet to be foamed. The continuous growth of the cell nuclei can obtain a foamed molded body with a cell structure. Among them, the above-mentioned "pressure relief" generally refers to reducing the pressure in the foaming cavity to below its critical point pressure, for example, reducing it to atmospheric pressure (i.e., normal pressure).

[0057] In some embodiments of the present application, the holding time in step 2) may be 30-90 minutes, for example, specifically 40 minutes, 45 minutes, 60 minutes, 80 minutes, or 90 minutes. In step 3), the foaming cavity is depressurized at a rate greater than or equal to 20 MPa / s to reduce the pressure in the foaming cavity to atmospheric pressure. The specific depressurization rate may be 25 MPa / s, 28 MPa / s, 30 MPa / s, 35 MPa / s, etc.

[0058] In some embodiments of the present application, after the supercritical foaming, the preparation method may further include: performing a hot pressing treatment. The hot pressing treatment may improve the surface flatness of the foamed sheet obtained by foaming and reduce the warping phenomenon. The processing temperature of the hot pressing treatment may be between Tg-30°C and Tg+30°C; wherein Tg represents the glass transition temperature of the foamed sheet, that is, the glass transition temperature of the polyester elastomer.

[0059] The preparation method of the above-mentioned grinding material in the present application is easy to operate and suitable for industrial mass production. The prepared grinding material is a foamed sheet of polyester elastomer, which has a high elastic recovery rate and high uniformity of thickness and pore size. It is particularly suitable for use in multilayer materials for flattening substrates, so that the grinding rate of the multilayer material on the substrate is stable, and has broad market application prospects.

[0060] The embodiment of the present application also provides a multilayer material, which includes a grinding layer, and the grinding layer is a foamed material of the above polyester elastomer. For the physical properties of the grinding layer material, please refer to the previous description of the present application.

[0061] In the implementation mode of the present application, as described above Figure 1A As shown, the multilayer material 100 may include a base layer 11, an adhesive layer 12, and the above-mentioned grinding layer 13 stacked in sequence. Figure 1B As shown, the multi-layer material 100 further includes a back adhesive layer 14 , which is located on a side of the base layer 11 away from the grinding layer 13 .

[0062] Among them, the base layer 11 mainly supports and buffers the grinding layer 13, ensuring the pressure balance at various locations on the grinding layer 13 during the working process of the multilayer material 100. The surface of the base layer 11 away from the grinding layer 13 is the adsorption surface of the multilayer material 100, which is used to ensure that the multilayer material 100 is attached to the substrate surface treatment device, such as attached to its working platform. In the case where there is a back adhesive layer 14 on the side of the base layer 11 away from the grinding layer 13, it is more conducive to ensuring that the multilayer material 100 adheres to the substrate surface treatment device more stably. The adhesive layer 12 is mainly used to achieve a good connection between the base layer 11 and the grinding layer 13, reducing the probability of interlayer separation during the working process of the multilayer material 100. The adhesive layer 12 can be specifically a solvent-free adhesive. The surface of the grinding layer 13 away from the base layer 11 is the working surface of the multilayer material 100, which is used to contact the surface to be processed of the substrate to be processed, so that the substrate obtains a flat surface under the mechanical action of the multilayer material 100 and the chemical action of the grinding working fluid.

[0063] In the embodiment of the present application, the thickness of the grinding layer 13 used in the multilayer material can be in the range of 0.3-4 mm. The thickness of the foamed sheet of the polyester elastomer is set in this range to ensure that the grinding layer 13 has a suitable hardness and compressibility, and give full play to the role of flattening the substrate. Specifically, the thickness of the grinding layer 13 can be 0.4 mm, 0.5 mm, 0.8 mm, 1.0 mm, 1.2 mm, 1.5 mm, 1.8 mm, 2.0 mm, 2.5 mm, 3.0 mm, 3.2 mm, 3.5 mm, 3.8 mm, etc.

[0064] The present application also provides an application of the above-mentioned grinding material or the above-mentioned multilayer material in the present application embodiment in the surface treatment of a substrate. The surface treatment of the substrate is specifically a flattening treatment of the surface of the substrate. The application can specifically be an application in a chemical mechanical polishing process.

[0065] The present application also provides a substrate surface treatment device, which includes the multilayer material described in the present application. The substrate surface treatment device can be used for planarization of the substrate surface. The substrate surface treatment device can be referred to as a "planarization treatment device" and can be used in a chemical mechanical polishing (CMP) process. The substrate can include but is not limited to a wafer, a semiconductor substrate, glass, metal, ceramic, optical device, etc.

[0066] Generally, the substrate surface treatment device may include a working platform and a grinding head suspended above the working platform, the surface of the working platform is paved with the multi-layer material, or the grinding head is mounted with the multi-layer material. The working platform may be referred to as a "working plate" in some cases.

[0067] See also Figure 2 , the substrate surface treatment device 200 provided in some embodiments of the present application includes a working platform 1, a multilayer material 100 laid on the surface of the working platform 1, a grinding head 2 suspended above the working platform 1, and a working liquid supply unit 4. The substrate 3 to be treated is installed on the grinding head 2, and its surface to be processed can contact with the multilayer material 100 during grinding, specifically, can contact with the grinding layer 13 of the multilayer material 100. The working platform 1 or the grinding head 2 can rotate in a clockwise or counterclockwise direction under the action of the electrode to start the treatment / processing process.

[0068] As described above in the present application, the multilayer material 100 can be adhered to the work platform 1, and its grinding layer 13 is away from the work platform 1. The multilayer material 100 can be specifically adhered by the adhesive layer 14 arranged on the side of the base layer 11 away from the grinding layer 13 to prevent the multilayer material 100 from moving randomly during the processing. The grinding head 2 is used to carry or clamp the substrate 3 to be processed, and press the substrate 3 to be processed against the multilayer material 100 with a certain pressure, so that the substrate 3 to be processed is located between the grinding head 2 and the multilayer material 100. The working liquid supply unit 4 is used to provide the working liquid, which is generally a chemical solution containing abrasive particles. During the processing of the substrate, the working liquid supply unit 4 can spray the working liquid onto the multilayer material 100, and the substrate 3 to be processed reacts chemically with the working liquid, and the surface is flattened under the mechanical friction with the multilayer material 100.

[0069] In some embodiments of the present application, the substrate surface treatment device 200 further includes a trimming unit 5. The trimming unit 5 is used to trim the multilayer material 100. During the processing of the substrate, the trimming unit 5 can be pressed against the multilayer material 100, and when the trimming unit 5 and the multilayer material 100 rub against each other, the debris and reactants on the surface of the multilayer material 100 are removed.

[0070] By using the substrate surface treatment device 200 with the multilayer material 100 according to the embodiment of the present application, the surface flattening treatment effect of the substrate 3 to be treated is good, and the device can work for a long time.

[0071] The technical solution of the embodiment of the present application is further explained below with multiple embodiments.

[0072] Example 1

[0073] A method for preparing a grinding layer material for a multi-layer material comprises the following steps:

[0074] Preparation of foaming profiles: Pre-dry the thermoplastic polyester elastomer (TPEE) particles with a hardness of 42D (composed of PTMEG polyether soft segment and PBT hard segment, with a melt index of 5.6g / 10min (190℃-2.16kg)) in a 90℃ oven for 12 hours, then add them to the feeding device of the extruder, pass nitrogen protection through the hopper, and feed by the sample's own weight. The extruder used is a single-screw sheet extruder, the segmented temperatures of the extruder barrel are 215℃, 210℃, and 220℃, the die temperature is 220℃, the extrusion rate is 0.25m / min, and the TPEE sheet prepared by the extruder has a width of 1.4 meters and a thickness of 2mm. After cooling, the extruded TPEE sheet is cut into 0.8m×0.8m square sheets, and its surface is cleaned with isopropanol and dried for use.

[0075] The TPEE square sheet prepared above was placed in a vacuum oven and annealed at 132°C for 5 hours, then the heating function of the vacuum oven was turned off and naturally cooled to 30°C. The sheet was then taken out and placed in a supercritical foaming kettle, and supercritical CO2 was introduced as a physical foaming agent to make the pressure in the foaming kettle reach a foaming pressure of 10MPa and the temperature reach a foaming temperature of 135°C. The foaming temperature and foaming pressure were maintained for 1.5 hours to achieve impregnation saturation. The foaming kettle was then depressurized at a rate of 28MPa / s to foam a TPEE foamed sheet with a microporous structure.

[0076] The density of the TPEE foam sheet was measured to be 0.67 g / cm 3 , the average cell diameter is 35 μm, and the hardness is 31 D. The standard deviation of thickness measured at different positions of the same TPEE foamed sheet is 6%.

[0077] Example 2

[0078] A preparation method for a grinding layer material for a multilayer material, which differs from Example 1 in that: when preparing a foaming profile, TPEE particles with a hardness of 60D are used as raw materials, the TPEE particles are composed of a PTMEG polyether soft segment and a PBT hard segment, and the melt index is 5.1g / 10min (190°C-2.16kg); the vacuum heat treatment temperature before supercritical foaming is 145°C; the foaming pressure of supercritical foaming is 12MPa, the foaming temperature is 125°C, and the pressure relief rate is 30MPa / s.

[0079] The density of the TPEE foam sheet prepared in Example 2 was measured to be 0.71 g / cm 3 , the average cell diameter is 38μm, and the hardness is 37D. The standard deviation of thickness measured at different positions of the same TPEE foamed sheet is 4%.

[0080] Example 3

[0081] A preparation method for a grinding layer material for a multilayer material, which differs from Example 2 in that the foaming agent used in supercritical foaming is supercritical N2, the foaming pressure is 10MPa, the foaming temperature is 157°C, the time for maintaining the foaming pressure and temperature is 1.5 hours, and the pressure relief rate is 30MPa / s.

[0082] The density of the TPEE foam sheet prepared in Example 3 was measured to be 0.67 g / cm 3 , the average cell diameter is 26 μm, and the hardness is 39 D. The standard deviation of thickness measured at different positions of the same TPEE foamed sheet is 2%.

[0083] In order to highlight the beneficial effects of the technical solution of the present application, the following comparative examples 1-2 are set.

[0084] Comparative Example 1

[0085] A method for preparing a grinding layer material for a multi-layer material comprises the following steps:

[0086] (1) 58 parts by weight of TDI (toluene diisocyanate, wherein the content of 2,4-toluene diisocyanate is 80 wt %, the content of 2,6-toluene diisocyanate is 20 wt %, and the NCO content in TDI is ≥48.0 wt %) and 100 parts by weight of PTMEG-650 (polytetramethylene glycol with a molecular weight of 650, a functionality of 2, and a hydroxyl value of 166.2-179.5 mgKOH / g) are reacted at 80° C. to obtain an NCO-terminated prepolymer, wherein the mass percentage of unreacted NCO groups in the prepolymer is 9.81 wt %.

[0087] (2) The NCO-terminated prepolymer is heated to 80° C. and vacuum degassed for 2 hours at a vacuum degree of 0.095 MPa to remove gases and small molecular compounds in the prepolymer; then, 2.4 parts by weight of a porogen (specifically, hollow polymer microspheres with a particle size D50 of 25 μm) is uniformly dispersed in 100 parts by weight of the above vacuum-degassed prepolymer by stirring, and vacuum degassed again at a vacuum degree of 0.095 MPa for 30 minutes to obtain a first mixture. 29.1 parts by weight of a diamine curing agent (specifically MOCA (3,3'-dichloro-4,4'-diphenylmethanediamine, amine value 7.4-7.6mmol / g) was added to the first mixture, and shear mixing was performed at high speed, and the obtained second mixture was poured into a cylindrical mold. The mold containing the material was pre-baked in an oven at 80°C for 30 minutes, and then the oven temperature was increased to 104°C within 30 minutes and cured for 16 hours. After the curing was completed, the oven heating function was turned off and the temperature was automatically cooled to room temperature. The sample taken out of the mold was a porous polyurethane elastomer, which could be used as a grinding layer for a multilayer material.

[0088] Among them, the density of the porous polyurethane elastomer prepared in Comparative Example 1 is 0.68 g / cm 3 , hardness is 40D.

[0089] Comparative Example 2

[0090] A preparation method for a grinding layer material for a multilayer material, which differs from Example 1 in that: when preparing a foaming profile, thermoplastic polyurethane (TPU) particles with a hardness of 95A are used as raw materials; no vacuum heat treatment is performed before supercritical foaming; the foaming pressure of the supercritical foaming is 10MPa, the foaming temperature is 125°C, the supercritical state is maintained for 3 hours, and the pressure relief rate is 30MPa / s.

[0091] The density of the TPU foam sheet obtained in Comparative Example 2 was 0.59 g / cm 3 , the average cell diameter is 41 μm, and the hardness is 30D. The standard deviation of the thickness measured at different positions of the same TPU foam sheet is 30%.

[0092] Comparative Example 3

[0093] A preparation method for a grinding layer material for a multi-layer material is disclosed, which is different from Example 1 in that the TPEE square sheet prepared in Example 1 is not subjected to vacuum heat treatment first, but is directly subjected to supercritical foaming.

[0094] The density of the TPEE foamed sheet in Comparative Example 3 was measured to be 0.67 g / cm 3, the average cell diameter is 36μm, and the hardness is 31D. The standard deviation of thickness measured at different positions of the same TPEE foamed sheet is 250%.

[0095] The grinding layer sheets prepared in the above embodiments and comparative examples were subjected to elastic recovery test and fatigue resistance test.

[0096] Among them, the elastic recovery rate test includes: taking samples on each grinding layer sheet respectively, obtaining a disc sample with a thickness of 2mm and a diameter of 1cm, recording the original thickness as H1, applying a 5kg weight, and then reading it after stabilizing for 60s, recording the thickness of the disc as H2, removing the 5kg weight, and then reading it after stabilizing for 60s, recording the thickness of the disc as H3, then the initial elastic recovery rate of each disc sample = (H3-H2) / (H1-H2)×100%.

[0097] Fatigue test: A 2 mm thick disc specimen was subjected to 50,000 fatigue tests in compression mode, with a deformation of 20% and a test frequency of 10 Hz.

[0098] After the fatigue test, a 5kg weight is applied to each disc sample, and the reading is taken after stabilization for 60s. The thickness of the disc is recorded as H4. After the 5kg weight is removed, the reading is taken after stabilization for 60s. The thickness of the disc is recorded as H5. After the fatigue test, the elastic recovery rate of each disc sample = (H5-H4) / (H1-H2)×100%.

[0099] Table 1 Elastic recovery rate of each grinding layer sheet before and after fatigue test

[0100] Initial elastic recovery rate (%) Elastic recovery rate after fatigue (%) Example 1 98 96 Example 2 98 98 Example 3 99 99 Comparative Example 1 98 57 Comparative Example 2 95 86

[0101] Table 1 above summarizes the elastic recovery rates of each grinding layer sheet before and after fatigue testing. As can be seen from Table 1, after up to 50,000 compression fatigue tests, the TPEE foam sheets of Examples 1-3 can still guarantee excellent elastic recovery rates, which are almost the same as the initial elastic recovery rates before fatigue testing; while the elastic recovery rates of the grinding layer sheets of Comparative Examples 1-2 are significantly reduced after multiple fatigue tests. This shows that the TPEE foam sheet provided in this application has good fatigue resistance, which enables the multi-layer polishing pad material prepared using it to maintain the same rebound level in the early and later stages of use, and maintain a stable polishing effect.

[0102] The grinding layer sheets prepared in the above embodiments and comparative examples were also subjected to DMA test to obtain their loss factors Tanδ at different temperatures. The relevant results are summarized in the following Tables 2 and Figure 3 middle.

[0103] Table 2

[0104]

[0105] From Table 2 and Figure 3 It can be seen that the Tanδ values ​​of the TPEE foamed sheets provided in the embodiments of the present application at multiple temperatures within the range of 25°C-85°C do not change much, and are very low, around 0.05. Accordingly, the lower the endogenous heat of each TPEE foamed sheet, the more stable the polishing rate of the multilayer polishing pad material made therefrom. However, the Tanδ values ​​of the thermosetting porous polyurethane materials of Comparative Examples 1-2 vary greatly at different temperatures. For example, the Tanδ values ​​of Comparative Example 1 within the temperature range of 25-55°C and the Tanδ values ​​of Comparative Example 2 within the temperature range of 60-85°C are both greater than 0.1, indicating that the endogenous heat of the material under the action of external force is very high, the elastic recovery is not good, and it cannot maintain good resilience in the entire temperature range of the foamed material, which is not conducive to its use in the multilayer material of the flattened substrate to maintain a stable grinding rate of the multilayer material.

[0106] In addition, the TPEE foamed sheet of each embodiment of the present application is used as a grinding layer to manufacture a multilayer material for flattening a substrate. Figure 1B As shown, the multilayer material includes a base layer 11, an adhesive layer 12 and a grinding layer 13 with a thickness of 2 mm, which are stacked in sequence. The base layer 11 is specifically a foamed buffer layer with a thickness of 1 mm and a compression rate of 25%. A back adhesive layer 14 with a thickness of 0.1 mm is also provided on the side of the base layer 11 away from the grinding layer 13, so that the obtained multilayer material can be adhered to the grinding test equipment through the back adhesive layer 14.

[0107] The test found that the rebound rate of the overall multilayer material did not change much in the early and late stages of use, and was both relatively high, and the polishing effect on the ground substrate (silicon wafer) was stable.

[0108] The above only expresses several exemplary embodiments of the present application, and the description is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present application. It should be pointed out that for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the present application, which all belong to the protection scope of the present application. Therefore, the protection scope of the patent of the present application shall be based on the attached claims.

[0109] It should be understood that the first, second and various numerical numbers involved in this document are only distinguished for the convenience of description and are not used to limit the scope of the present application.

[0110] In this application, "and / or" describes the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone, where A and B can be singular or plural. The character " / " generally indicates that the associated objects are in an "or" relationship.

[0111] In this application, "at least one" means one or more, and "more than one" means greater than or equal to two. "At least one of the following" or similar expressions refers to any combination of these items, including any combination of single or plural items. For example, "at least one of a, b, or c", or "at least one of a, b, and c", can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, c can be single or multiple, respectively.

Claims

1. A grinding material for substrate surface treatment, characterized in that: The grinding material is a foamed sheet of polyester elastomer, and the loss factor of the grinding material at any temperature within the range of 25-85° C. is less than 0.

1.

2. The abrasive material according to claim 1, characterized in that The loss factor of the grinding material at any temperature within the range of 25-85° C. is less than or equal to 0.

08.

3. The abrasive material according to claim 1 or 2, characterized in that: The elastic recovery rate of the grinding material is above 90%.

4. The grinding material according to any one of claims 1 to 3, characterized in that After the grinding material is subjected to 50,000 compression fatigue tests with a deformation amount of 20%, the elastic recovery rate is above 90%.

5. The grinding material according to any one of claims 1 to 4, characterized in that: The relative standard deviation of the thickness of the same foamed sheet does not exceed 10%.

6. The abrasive material according to any one of claims 1 to 5, characterized in that: The average pore size of the grinding material is 5-50 μm.

7. The abrasive material according to any one of claims 1 to 6, characterized in that: The surface porosity of the grinding material is in the range of 20%-80%.

8. The abrasive material according to any one of claims 1 to 7, characterized in that: The density of the grinding material is 0.3-1.0 g / cm 3 .

9. The abrasive material according to any one of claims 1 to 8, characterized in that: The Shore hardness of the abrasive material at 25° C. is in the range of 15A-60D.

10. The grinding material according to any one of claims 1 to 9, characterized in that: The polyester elastomer comprises a polyester hard segment and a polyether soft segment, wherein the polyester hard segment is selected from one or more of polyethylene terephthalate, polybutylene terephthalate, and polypropylene terephthalate; and the polyether soft segment comprises one or more of a polytetrahydrofuran diol segment, a polyoxypropylene diol segment, and a polyoxyethylene diol segment.

11. The abrasive material according to any one of claims 1 to 10, characterized in that: The grinding material is obtained by subjecting a formed sheet containing the polyester elastomer to vacuum heat treatment and then to supercritical foaming.

12. A method for preparing a grinding material, characterized in that: The following steps are involved: forming a polyester elastomer into a sheet for foaming; The foaming sheet is subjected to vacuum heat treatment and then supercritical foaming to obtain a grinding material; wherein the grinding material is a foaming sheet of a polyester elastomer, and the loss factor of the grinding material at any temperature within the range of 25-85°C is less than 0.

1.

13. The preparation method according to claim 12, characterized in that: The vacuum heat treatment temperature is between T m -20℃ to T m ℃, the treatment time is 1-10 hours; among which, T m represents the melting point of the polyester elastomer.

14. A multilayer material, characterized in that It comprises a base layer, an adhesive layer and a grinding layer which are stacked in sequence, and the grinding layer comprises the grinding material according to any one of claims 1 to 11.

15. The multilayer material according to claim 14, characterized in that A back adhesive layer is also provided on the side of the base layer away from the grinding layer.

16. The multilayer material according to claim 14 or 15, characterized in that The thickness of the grinding layer is 0.3 mm-4 mm.

17. Use of the abrasive material according to any one of claims 1 to 11, or the multilayer material according to any one of claims 14 to 16 in substrate surface treatment.

18. A substrate surface treatment device, characterized in that: The substrate surface treatment device carries the multilayer material according to any one of claims 14-16.

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