CN115771109A - Method for preparing novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel through in-situ reaction - Google Patents
Method for preparing novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel through in-situ reaction Download PDFInfo
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Abstract
The invention belongs to the field of grinding wheel preparation, and discloses a method for preparing a novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel by in-situ reaction, which comprises the following components in percentage by mass: a1 powder:
carbon nitride powder:
ti powder:
cr powder:
fe powder:
the invention overcomes the disadvantage of poor wettability of the original ceramic bond and metal, selects the carbon nitride material with low cost, prepares the novel A1-based ceramic composite bond by the in-situ reaction sintering technology, develops the novel aluminum-based ceramic composite bond silicon carbide thinning grinding wheel, has sharp grinding performance, can be simultaneously applied to processing the silicon surface and the carbon surface of the silicon carbide wafer, has long service life and low production cost.
Description
Technical Field
The invention relates to the field of grinding wheel preparation, in particular to a method for preparing a novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel through in-situ reaction.
Background
With the rapid development of modern industries, especially the rapid development of mechanical and electronic industries, grinding tools for fine grinding and semi-fine grinding are more and more widely applied. As an important substrate material in the semiconductor industry, the silicon carbide single crystal has excellent thermal and electrical properties and has wide application prospects in the field of high-temperature, high-frequency and high-power integrated electronic devices. The processing precision of the silicon carbide substrate directly affects the performance of the device, so the requirements of epitaxial application on the surface quality of the silicon carbide wafer are extremely strict. Silicon carbide has high hardness, large brittleness and stable chemical property, and the traditional processing method is not completely applicable. The silicon carbide wafer has a carbon surface and a silicon surface which are both difficult to grind compared with the traditional monocrystalline silicon wafer and are limited by the processing technology, and the processing efficiency of the silicon carbide wafer with high surface quality is extremely low at present. In the process of thinning the silicon carbide wafer, firstly, coarse grinding treatment is carried out, and at present, a ceramic bond diamond grinding tool with good self-sharpening performance is mainly adopted. The main problems of the prior art are that the strength of the ceramic bond diamond grinding tool is low, the holding force of the bond to the diamond is relatively low, and the grinding efficiency and the service life are short. The silicon carbide material has higher hardness and is particularly wear-resistant, so that the diamond grinding tool is required to have higher strength, and the holding force of the bonding agent to the diamond is good.
At present, the ceramic bond mainly adopts low-melting-point ceramic prepared and smelted by various oxides, and has the prominent defects of poor wettability with diamond, high brittleness and the like although the self-sharpening property is better. In response to the disadvantage of ceramic binders, many researchers have considered the addition of metals to ceramic binders to construct composite metal/ceramic composite binders. The composite bond grinding tool is expected to have the characteristics of high self-sharpening property, high grinding efficiency and easiness in trimming of the ceramic grinding tool, and also has the characteristics of high strength, high hardness, high toughness and long service life of the metal bond. For example, the patent "a ceramic-metal bond diamond grinding tool and its preparation method (CN 102152248B)" proposes a ceramic bond based on a small amount of metal bond, and a small amount of metal (Ti 1-10%, al 1-5%) is added to the formula of the bond.
The research on the metal/ceramic composite bonding agent diamond grinding tool has already provided a good research foundation. However, the matrix of the diamond tool in the market still mainly uses a pure metal bond or a ceramic bond, and the practical application of the composite bond is almost zero. The underlying reason is that simple mixing of the two binders does not result in a benign and appropriate chemical reaction between the two, which results in poor wetting or bonding of the metal to the ceramic binder. The inherent disadvantages of the respective bonds have not been overcome and remain, which has resulted in the actual grinding performance of the bonded composite abrasive article failing to meet the intended objectives of the study.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing a novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel by in-situ reaction.
The principle of the technology is that according to the requirement of material design, proper reactants (gas phase, liquid phase or powder solid phase) are selected, and a reinforcing phase with very fine size and uniform distribution is generated in situ by virtue of chemical reaction between base metal or alloy and the base metal or alloy at proper temperature. The in-situ reaction under the patent has the advantages that the carbon nitride has higher reaction activity, is easy to react with aluminum, can react completely and quickly at the temperature of the invention, and has the outstanding advantage of quick reaction. In a short reaction time, the high-activity carbon nitride is beneficial to inhibiting the etching of aluminum to the diamond, and the diamond can be effectively protected from being damaged in the sintering process. The schematic of the microstructure is shown in FIG. 1, in which the reinforcing phase is evident. As can be seen from fig. 2, aluminum reacts with carbon nitride in situ and forms Al and Al4C3 ceramics. Further, carbon nitride adsorbs a small amount of O2, and Al2O3 is generated by the reaction of aluminum with O2. The reaction formula is as follows:
8Al+C3N4＝Al4C3+4AlN (1)
2Al+1.5O2＝Al2O3 (2)
the newly generated ceramic particles such as AlN and the like have good wettability with aluminum, and the bonding between the ceramic particles such as AlN and the like and an aluminum substrate is better due to a clean interface, which is obviously different from the method that metal is directly added into a ceramic bonding agent in the background technology to construct a metal ceramic composite bonding agent.
The invention aims to overcome the defects of the ceramic bond and provide a novel silicon carbide thinning grinding wheel with an aluminum-based ceramic composite bond, which has the advantages of sharp grinding, strong holding force, long service life and low cost, and a preparation method thereof.
The method for preparing the novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel by in-situ reaction adopts the following technical scheme:
a method for preparing a novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel through in-situ reaction comprises the following components in percentage by mass: a1 powder:
carbon nitride powder:
ti powder:
cr powder:
fe powder:
further, as a partial substitute for the above A1, the above metal binder may be further added
(weight percent) one or two of Ti, cr and Fe.
Further, the A1, ti, cr and Fe powders have a purity of 99% or more and a particle size of 200-400 mesh.
Further, the carbon nitride powder is prepared by taking melamine powder as a raw material, heating the raw material at a speed of 5 ℃ per minute in a muffle furnace, carrying out thermal decomposition at 550 ℃ for 4 hours to obtain a block product, carrying out ball milling and grinding, and sieving the block product through a metal sieve to obtain different particle sizes (150-300 meshes).
Further, including emery wheel base member and abrasive brick piece, its characterized in that: the abrasive material block consists of a bonding agent and diamond, and the mass ratio of the bonding agent to the diamond is 80:20.
further, the diamond has a particle size of 2000 mesh.
Further, the method comprises the following steps:
(1) Weighing raw material powder such as aluminum powder, carbon nitride, alternative metal and the like according to different raw material proportions, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain the finally required mixed powder.
(2) And (3) loading the prepared mixed powder material into a graphite die, adopting a high-temperature hot-pressing sintering method, using a forming pressure of 60-100KN and a sintering temperature of 600-650 ℃, keeping the temperature and pressure for 8-15 minutes, naturally cooling, and demoulding to obtain a sintered abrasive block.
(3) And adhering the obtained abrasive block on a grinding wheel matrix, and machining according to the shape and the size of the grinding wheel to reach the specification and the size of a finished product to obtain the aluminum-based binder diamond grinding wheel.
In summary, the invention includes at least one of the following beneficial technical effects: the invention overcomes the disadvantage of poor wettability of the original ceramic bond and metal, selects the carbon nitride material with low cost, prepares the novel A1-based ceramic composite bond by the in-situ reaction sintering technology, develops the novel aluminum-based ceramic composite bond silicon carbide thinning grinding wheel, has sharp grinding performance, can be simultaneously applied to processing the silicon surface and the carbon surface of the silicon carbide wafer, has long service life and low production cost.
Drawings
FIG. 1 is a schematic view of the texture of a grinding wheel.
FIG. 2 is an XRD pattern of an example prepared grinding wheel.
FIG. 3 is a schematic view of the structure of the finished grinding wheel.
Detailed Description
The present invention is described in further detail below with reference to figures 1-3.
The embodiment of the invention discloses a method for preparing a novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel by in-situ reaction, which comprises the following steps:
example 1
The novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel comprises a grinding wheel base body and a grinding block, wherein the grinding block consists of a bonding agent and diamonds, and the mass ratio of the bonding agent to the diamonds is 80:20, the bonding agent is prepared from the following raw materials in percentage by mass: a1 powder: 70%, carbon nitride powder: 30 percent. The granularity of the A1 powder, the granularity of the carbon nitride powder and the granularity of the diamond are 200 meshes, 200 meshes and 2000#, respectively.
The carbon nitride is prepared by taking industrial-grade (purity is equal to or greater than 99.8%) melamine powder as a raw material, carrying out pyrolysis in a muffle furnace at a temperature rise rate of 5 ℃ per minute for 4 hours at 550 ℃ to obtain a massive product, carrying out ball milling and grinding on the massive product, and sieving the massive product through a metal sieve to obtain 200-mesh powder.
The preparation method of the aluminum-based binder diamond grinding wheel comprises the following steps:
a) Weighing aluminum powder and carbon nitride powder according to the raw material ratio, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain finally required mixed powder;
b) Loading the mixture obtained in the step a) into a graphite mold, and placing the graphite mold into a hot-pressing sintering machine for pressing and sintering in an air atmosphere, wherein the method specifically comprises the following steps: heating to 630 ℃ at the speed of 50 ℃/min, keeping the forming pressure of 60KN for 8min, naturally cooling, and demoulding to obtain the abrasive block;
c) And d, bonding the abrasive block obtained in the step b on a grinding wheel base body, and processing to reach the specification and the size of a finished product to obtain the aluminum-based bonding agent diamond grinding wheel.
Example 2
The novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel comprises a grinding wheel base body and a grinding block, wherein the grinding block consists of a bonding agent and diamonds, the mass ratio of the bonding agent to the diamonds is 80, and the bonding agent is prepared from the following raw materials in percentage by mass: a1 powder: 60%, ti powder: 5%, carbon nitride powder: 35 percent. The granularity of the A1 powder, the Ti powder, the carbon nitride powder and the diamond is 200 meshes, 300 meshes, 150 meshes and 2000#, respectively.
The carbon nitride is a block product obtained by pyrolysis of industrial grade (purity ≧ 99.8%) melamine powder as raw material in a muffle furnace at a temperature rise rate of 5 degrees/min and at a temperature of 550 degrees for 4 hours. After ball milling and grinding, the powder is sieved by a metal sieve to obtain 150-mesh powder.
The preparation method of the aluminum-based binder diamond grinding wheel comprises the following steps:
a) Weighing aluminum powder, titanium powder and carbon nitride powder according to the raw material ratio, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain the finally required mixed powder;
b) Loading the mixture obtained in the step a) into a graphite mold, and placing the graphite mold into a hot-pressing sintering machine for pressing and sintering in an air atmosphere, wherein the method specifically comprises the following steps: heating to 650 ℃ at the speed of 50 ℃/min, keeping the molding pressure of 80KN for 10min, naturally cooling, and demolding to obtain the abrasive block;
c) And d, bonding the abrasive block obtained in the step b on a grinding wheel base body, and processing to reach the specification and the size of a finished product to obtain the aluminum-based bonding agent diamond grinding wheel.
Example 3
The novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel comprises a grinding wheel base body and a grinding block, wherein the grinding block consists of a bonding agent and diamonds, the mass ratio of the bonding agent to the diamonds is 80, and the bonding agent is prepared from the following raw materials in percentage by mass: a1 powder: 50%, ti powder: 10%, carbon nitride powder: 40 percent. The granularity of the A1 powder, the Ti powder, the carbon nitride powder and the diamond is 300 meshes, 200 meshes, 300 meshes and 2000#, respectively.
The carbon nitride is prepared by using industrial-grade (purity is not less than 99.8%) melamine powder as a raw material, performing pyrolysis in a muffle furnace at a temperature rise rate of 5 ℃ per minute for 4 hours at a temperature of 550 ℃ to obtain a block product, performing ball milling and grinding, and sieving through a metal sieve to obtain 300-mesh powder.
The preparation method of the aluminum-based binder diamond grinding wheel comprises the following steps:
a) Weighing aluminum powder, titanium powder and carbon nitride powder according to the raw material ratio, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain the finally required mixed powder;
b) Loading the mixture obtained in the step a) into a graphite die, and placing the graphite die into a hot-pressing sintering machine for pressing and sintering in an air atmosphere, wherein the method specifically comprises the following steps: heating to 630 ℃ at the speed of 50 ℃/min, keeping the forming pressure of 80KN for 12min, naturally cooling, and demoulding to obtain the abrasive block;
c) And d, bonding the abrasive block obtained in the step b on a grinding wheel base body, and processing to reach the specification and the size of a finished product to obtain the aluminum-based bonding agent diamond grinding wheel.
Example 4
The novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel comprises a grinding wheel base body and a grinding block, wherein the grinding block consists of a bonding agent and diamonds, and the mass ratio of the bonding agent to the diamonds is 80:20, the bonding agent is prepared from the following raw materials in percentage by mass: a1 powder: 75%, cr powder: 5%, carbon nitride powder: 20 percent. The granularity of the A1 powder, the Cr powder, the carbon nitride powder and the diamond is 300 meshes, 400 meshes, 200 meshes and 2000#, respectively.
The carbon nitride is a block product obtained by pyrolysis of industrial-grade (purity ≧ 99.8%) melamine powder as a raw material in a muffle furnace at a temperature rise rate of 5 degrees/min and at 550 degrees for 4 hours. After ball milling and grinding, the powder is sieved by a metal sieve to obtain 200-mesh powder.
The preparation method of the aluminum-based binder diamond grinding wheel comprises the following steps:
a) Weighing aluminum powder, chromium powder and carbon nitride powder according to the raw material ratio, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain the finally required mixed powder;
b) Loading the mixture obtained in the step a) into a graphite mold, and placing the graphite mold into a hot-pressing sintering machine for pressing and sintering in an air atmosphere, wherein the method specifically comprises the following steps: heating to 630 ℃ at the speed of 30 ℃/min, keeping the forming pressure of 100KN for 15min, naturally cooling, and demolding to obtain the abrasive block;
c) And d, bonding the abrasive block obtained in the step b on a grinding wheel base body, and processing to reach the specification and the size of a finished product to obtain the aluminum-based bonding agent diamond grinding wheel.
Example 5
The novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel comprises a grinding wheel base body and a grinding block, wherein the grinding block consists of a bonding agent and diamonds, and the mass ratio of the bonding agent to the diamonds is 80:20, the bonding agent is prepared from the following raw materials in percentage by mass: a1 powder: 55%, fe powder: 5%, carbon nitride powder: 40 percent. The granularity of the A1 powder, the Fe powder, the carbon nitride powder and the diamond is 300 meshes, 200 meshes and 2000#, respectively.
The carbon nitride is prepared by taking industrial-grade (purity is equal to or greater than 99.8%) melamine powder as a raw material, carrying out pyrolysis in a muffle furnace at a temperature rise rate of 5 ℃ per minute for 4 hours at 550 ℃ to obtain a massive product, carrying out ball milling and grinding on the massive product, and sieving the massive product through a metal sieve to obtain 200-mesh powder.
The preparation method of the aluminum-based binder diamond grinding wheel comprises the following steps:
a) Weighing aluminum powder, iron powder and carbon nitride powder according to the raw material ratio, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain the finally required mixed powder;
b) Loading the mixture obtained in the step a) into a graphite mold, and placing the graphite mold into a hot-pressing sintering machine for pressing and sintering in an air atmosphere, wherein the method specifically comprises the following steps: heating to 650 ℃ at the speed of 30 ℃/min, keeping the forming pressure of 100KN for 15min, naturally cooling, and demolding to obtain the abrasive block;
c) And d, bonding the abrasive block obtained in the step b on a grinding wheel base body, and processing to a finished product specification size to obtain the aluminum-based bonding agent diamond grinding wheel.
Example 6
The novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel of the embodiment comprises a grinding wheel base body and a grinding material block, wherein the grinding material block comprises a bonding agent and diamonds, and the bonding agent and the diamonds have a mass ratio of 80:20, the bonding agent is prepared from the following raw materials in percentage by mass: a1 powder: 80%, carbon nitride powder: 20 percent. The granularity of the A1 powder, the granularity of the carbon nitride powder and the granularity of the diamond are respectively 300 meshes, 200 meshes and 2000#.
The carbon nitride is prepared by using industrial-grade (purity is not less than 99.8%) melamine powder as a raw material, performing pyrolysis in a muffle furnace at a temperature rise rate of 5 ℃ per minute for 4 hours at a temperature of 550 ℃ to obtain a block product, performing ball milling and grinding, and sieving through a metal sieve to obtain 200-mesh powder.
The preparation method of the aluminum-based binder diamond grinding wheel comprises the following steps:
a) Weighing aluminum powder and carbon nitride powder according to the raw material ratio, mixing for 2 hours by using a three-dimensional mixer, sieving to obtain mixed powder, mixing the obtained mixed powder and diamond particles for 1 hour, and sieving to obtain finally required mixed powder;
b) Loading the mixture obtained in the step a) into a graphite mold, and placing the graphite mold into a hot-pressing sintering machine for pressing and sintering in an air atmosphere, wherein the method specifically comprises the following steps: heating to 600 ℃ at the speed of 30 ℃/min, keeping the forming pressure of 100KN for 15min, naturally cooling, and demolding to obtain the abrasive block;
c) And d, bonding the abrasive block obtained in the step b on a grinding wheel base body, and processing to a finished product specification size to obtain the aluminum-based bonding agent diamond grinding wheel.
The application condition of the novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel in silicon carbide wafer thinning processing is shown in table 2.
Table 1 mass content and particle size of the binder raw materials.
Table 2 grinding performance of the examples and the comparative examples.
Compared with the common ceramic bond grinding wheel for thinning silicon carbide, the novel aluminum-based ceramic composite bond grinding wheel manufactured by the method generates the reinforcing phase by the in-situ reaction of carbon nitride and metal, the holding force of the bonding agent on the grinding material is greatly improved, and the application indexes of the embodiment, such as service life (grinding ratio), sharpness (grinding current), processing quality and the like, are superior to those of the comparative example. In six groups of embodiments, in the embodiments 2 to 5, because of additionally adding replacement metal components such as Ti, cr, fe and the like, the added carbon nitride and metal react more fully, the generated fine nitride or carbide can play a role in strengthening and toughening, the performance of the bonding agent is further improved, and each application index of the bonding agent is obviously superior to that of the embodiments 1 and 6 without adding the replacement metal components.
The above are all preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (7)
1. The in-situ reaction preparation of the novel aluminum-based ceramic composite binder is characterized in that: the composite material comprises the following components in percentage by mass: a1 powder:
carbon nitride powder:
ti powder: 0
Cr powder:
fe powder:
2. the in-situ reaction preparation novel aluminum-based ceramic composite binder as claimed in claim 1, wherein: as a partial alternative to A1, the metal binder may further contain
(weight percent) one or two of Ti, cr and Fe.
3. The in-situ reaction preparation novel aluminum-based ceramic composite binder as claimed in claim 1, wherein: the A1, ti, cr and Fe powder has a purity of 99% or more and a particle size of 200-400 meshes.
4. The in-situ reaction preparation novel aluminum-based ceramic composite binder as claimed in claim 1, wherein: the carbon nitride powder is prepared by taking melamine powder as a raw material, heating the raw material at a speed of 5 ℃ per minute in a muffle furnace, carrying out thermal decomposition at 550 ℃ for 4 hours to obtain a block product, carrying out ball milling and grinding, and sieving the block product by a metal sieve to obtain different particle sizes (150-300 meshes).
5. The in-situ reaction preparation novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel as claimed in claim 1, which comprises a grinding wheel base body and a grinding block, and is characterized in that: the abrasive material block consists of a bonding agent and diamond, and the mass ratio of the bonding agent to the diamond is 80.
6. The in-situ reaction prepared novel aluminum-based ceramic composite binding agent silicon carbide thinning grinding wheel according to claim 5, characterized in that: the diamond particle size is 2000 mesh.
7. The method for preparing the novel aluminum-based ceramic composite bonding agent silicon carbide thinning grinding wheel according to the claim 1, which is characterized in that: the method comprises the following steps: (1) Weighing raw material powder of aluminum powder, carbon nitride, alternative metal and the like according to different raw material proportions, mixing for 2 hours by using a three-dimensional mixer, and sieving to obtain mixed powder. Mixing the obtained mixed powder and the diamond particles for 1 hour, and sieving to obtain the finally required mixed powder.
(2) And (3) loading the prepared mixed powder material into a graphite die, adopting a high-temperature hot-pressing sintering method, using a forming pressure of 60-100KN and a sintering temperature of 600-650 ℃, keeping the temperature and pressure for 8-15 minutes, naturally cooling, and demoulding to obtain a sintered abrasive block.
(3) And adhering the obtained abrasive block on a grinding wheel matrix, and machining according to the shape and the size of the grinding wheel to reach the specification and the size of a finished product to obtain the aluminum-based binder diamond grinding wheel.
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