CN116477956A - Precise machining process and formula for large-sized structural ceramic - Google Patents

Precise machining process and formula for large-sized structural ceramic Download PDF

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Publication number
CN116477956A
CN116477956A CN202310466991.1A CN202310466991A CN116477956A CN 116477956 A CN116477956 A CN 116477956A CN 202310466991 A CN202310466991 A CN 202310466991A CN 116477956 A CN116477956 A CN 116477956A
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powder
grinding
ceramic
agent
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CN202310466991.1A
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Chinese (zh)
Inventor
黄明东
赵韦人
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Guangdong Fengxin Intelligent Technology Co ltd
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Guangdong Fengxin Intelligent Technology Co ltd
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Priority to CN202310466991.1A priority Critical patent/CN116477956A/en
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B11/00—Machines or devices designed for grinding spherical surfaces or parts of spherical surfaces on work; Accessories therefor
    • B24B11/02—Machines or devices designed for grinding spherical surfaces or parts of spherical surfaces on work; Accessories therefor for grinding balls
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/02—Lapping machines or devices; Accessories designed for working surfaces of revolution
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  • Physics & Mathematics (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)

Abstract

The invention discloses a precise processing technology and a formula of large-sized structural ceramics, wherein the preparation raw materials comprise, by weight, 47-65 parts of a mixture, 3-7 parts of a dispersing agent, 2-5 parts of an active agent, 6-9 parts of a binding agent, 1-5 parts of a catalyst, 7-13 parts of an auxiliary agent, 8-11 parts of an abrasive and 2-6 parts of an abrasive; in the sintering process, a proper amount of binding agent is added, so that the ceramic ball blank is more compact, and as the nitrogen pressure is increased, pores or cracks in the blank are closed and disappear under the effect of nitrogen pressure increase, the internal structure is more compact, and the mechanical property is obviously improved; in the processing process of the ceramic ball, the ceramic bearing is precisely manufactured and reinforced in service life and quality.

Description

Precise machining process and formula for large-sized structural ceramic
Technical Field
The present invention relates toCeramic materialThe processing field, in particular to a precise processing technology and a formulation of large-scale structural ceramics.
Background
At present, the requirements on the bearing capacity and the processing precision of a plurality of machines are higher and higher, the living environment is more diversified, a plurality of machine parts are also required to be updated gradually along with the progress of science and technology,the ceramic appliances are used more to replace the metal appliancesCeramic materials as nonmetallic engineering materials are taking an increasingly important place in the development of modern mechanical applications,Especiallyin the aspect of manufacturing ceramic balls as rolling bodies of the bearings, the ceramic ball bearings with high performance can be manufactured, the most main components of the ceramic ball bearings are the ceramic ball rolling bodies, the ceramic balls are the keys for improving the service life and the rotating speed of the ceramic bearings, the quality of the ceramic balls directly influences the performance of the bearings, the forming of ceramic ball blanks influences the processing efficiency and the quality of finished products, and the existing ceramic ball blank finished products have the characteristics of high temperature resistance, wear resistance and the like, but have poor common antibacterial performance, poor oxidation resistance and the surface mechanical strength of ceramic structuresAnd uniformity of allThe quality of the product is poor,in particular, in the case of ceramic manufacture, the antioxidants added thereto are not uniformly distributed The ceramic is integrated so that the integral performance of the ceramic is greatly affected, although the ceramic is re-treated on the later surface of the ceramic Is sprayed with an oxidation-resistant and wear-resistant coating, but the overall physical and chemical properties of the ceramic are mostly determined by the manufacturing process and the chemical properties The influence of the formulation is such that,these areAll problems will occurThe overall service life of the ceramic structure is severely affected.
Disclosure of Invention
The invention provides a precise processing technology and a formula of large-sized structural ceramics for solving the technical problems.
The technical scheme of the invention is realized as follows:
the precise machining recipe for large structural ceramic includes the materials including mixture 47-65 weight portions, dispersant 3-7 weight portions, activator 2-5 weight portions, binder 6-9 weight portions, catalyst 1-5 weight portions, assistant 7-13 weight portions, grinding agent 8-11 weight portions and grinding material 2-6 weight portions.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
The process for precisely machining large structural ceramic includes the following steps:
s1: taking part of raw materials silicon dioxide and carbon powder, and carbonizing, reducing and nitriding SiO 2 The mixture with C powder enters N 2 And heating at 1200deg.C, wherein the reaction is performed in two steps, siO 2 Reducing under the action of C powder to generate Si;
s2: then Si and N are mixed at 1100-1500 DEG C 2 Reaction to produce Si 3 N 4 The general reaction formula is: 3SiO 2 +6C+2N 2 ＝Si 3 N 4 +6CO, sufficient carbon to ensure SiO is added to make the reaction more complete 2 Completely reacting; s3: and SiO during the manufacturing process 2 Si is added into the mixed powder of-C 3 N 4 After 1300 ℃ heating treatment, the obtained silicon nitride powder crystal is different from the powder crystal obtained by simple carbonization and reduction, and the main shape of the crystal is sharp.
The preparation process of the silicon nitride ceramic comprises the following steps:
s1: grinding, in order to fully react, grinding silicon carbide forming crystals and caking, wherein the product purity is low, the particles are large, and the powder is crushed and ground, so that the particles are more compact and uniform;
s2: adding composite abrasive, preparing silicon nitride powder into secondary granules with the granularity of about 0.1mm by using a cold isostatic pressing method, improving the pressing performance and flowability of the powder, wherein the cold isostatic pressing method is carried out in a closed environment, so that impurities can be prevented from being mixed into the powder, the integral quality after molding is damaged, and the cold isostatic pressing method is selected to complete granulation in order to ensure the purity of the powder and the quality after processing;
s3, the silicon nitride ceramic powder compounding technology generally adopts a liquid-powder phase mixing method, absolute ethyl alcohol is used as a dispersion medium, polyethylene glycol is used as a dispersion auxiliary agent, and ultrasonic waves are used for treating liquid phase call objects to finish mixing ingredients;
s4, adding the mixture, the binding agent and deionized water according to the proportion, granulating to improve the fluidity and the compressibility of the silicon nitride powder, and adding the powder after granulating the mixture into a metal cavity through dry-press forming and cold isostatic pressing to improve the strength;
s5, adding a dispersing agent to enable the particles to be ionized into ions and then to be adsorbed on the surfaces of the particles, forming an electric double layer structure on the surfaces of the particles, improving the surface charge density of the particles, overcoming the van der Waals attractive force among the particles through the effect of the same charge repulsive force on the surfaces, realizing the dispersing effect, enabling the high-purity silicon nitride powder to be a barren material, and ensuring that the formed spherical blank has enough strength and is formed by adding an active agent to change the characteristics of powder crystals, wherein the surface performance is very weak and the polymerization difficulty is high;
s6: the quality detection is carried out on the ball blank, the ball performance of the blank which is not finished in quality detection does not meet the processing standard, the blank is required to be sintered to strengthen the strength of the blank, after the sintering is finished, the ceramic ball blank is more compact, the density is increased, the strength is also increased along with the increase, and the preparation is made for the grinding processing of the ceramic ball;
s7: before preventing the decomposition of silicon nitride, embedding the blank ball into mixed powder of silicon nitride and boron nitride with the similar composition to that of the blank ball, wherein the mixed powder forms a gas phase balance environment on the surface of the ball blank to prevent the decomposition of silicon nitride;
s8: in the sintering process, the temperature is controlled within the range of 1700-2000 ℃, and the silicon nitride can undergo decomposition reaction at the high temperature of 1900 ℃: si (Si) 3 N 4 ＝3Si+2N 2 In the sintering process, the process is carried out under certain nitrogen pressure, so that the silicon nitride is not decomposed, the nitrogen can prevent the decomposition of the silicon nitride and can also play a role in densification of density, and better blank quality is obtained;
s9: the auxiliary agent is added during the re-sintering, and the density after the re-sintering is more than 90 percent, even can reach 99 percent. And shrinkage is generally less than 6.5%.
The processing process of the silicon nitride ceramic comprises the following steps:
s1: the method comprises the steps of firing the formed silicon nitride ceramic balls, carrying out quality inspection and fluorescent flaw detection on blank balls, selecting extremely large balls and extremely small balls, carrying out rough grinding processing on the blank balls to remove 95% of the ceramic ball allowance, and ensuring that the processing allowance range of the blank balls is not excessively large and is within the range of 0.3-0.5mm so as to ensure that the processing can be carried out;
s2: after rough grinding and fine grinding, the granularity of the grinding material is 20-40 mu m, an oil agent or water agent grinding liquid is added, the rotating speed of a grinding plate is 48-120r/min, the pressure is 2-3Mpa, fine grinding is carried out, the ceramic ball has good appearance, but the surface of the processed ball is still rough, and the precision is lower;
s3: adding a compound abrasive, wherein the abrasive grain size is 1-3.5Mm, adding an oil or water agent grinding liquid, and performing preliminary grinding processing under the pressure of 1-2.5Mpa at the rotating speed of 25-60r/min, so as to improve the surface quality and processing precision of the ceramic balls and eliminate the stress on the surfaces of the ceramic balls;
s4: in the last step, compound abrasive is added, the granularity of the abrasive is less than 1 mu m, oil or water agent grinding liquid is added, the rotating speed of a grinding plate is 15-20r/min, the pressure is 1-3Mpa, the lapping processing is carried out, the grinding rotating speed is lower, the pressure cannot be too high, and the lapping steady state and the ball structure and the surface quality are not damaged;
s5: after lapping, the ceramic ball basically reaches the required precision, and finally polishing the ceramic ball to continuously improve the machining precision, and further improving the precision of the polished ball to finish the precision machining of the ceramic ball.
The beneficial effects are that:
according to the preparation process of the ceramic balls, the dispersing agent is added in the preparation process of the ceramic balls,to make ceramic at When the embryo is manufactured, the components are distributed more uniformly, the integral strength of the ceramic is greatly increased, and the dispersing agent ensures thatThe particles are ionized into ions and then adsorbed on the surfaces of the particles, the surface of the particles forms an electric double layer structure, so that the surface charge density of the particles is improved, the van der Waals attraction between the particles is overcome through the repulsive force action of the same charge on the surfaces, the characteristics of powder crystals are changed by adding an active agent, the characteristics of the powder crystals are changed by ensuring that the formed spherical blank has enough strength, the forming rate and the forming strength are improved, and the uniformity and the strength of the texture of the formed spherical blank are ensured; in the sintering process, a proper amount of binding agent is added, so that the ceramic ball blank is more compact, the density is increased, the strength is also increased along with the increase of the nitrogen pressure, the density of the blank ball is increased under the mutual alternating action of the blank ball, and air holes or cracks in the blank are closed and disappear under the effect of the nitrogen pressure increase, so that the internal structure is more compact, and the mechanical property is obviously improved; in the processing process of the ceramic ball, the ceramic bearing is precisely manufactured and reinforced in service life and quality.
Drawings
FIG. 1 is a workflow of a precision machining process for large structural ceramics according to the present invention.
Detailed Description
As shown in figure 1, the preparation raw materials of the large-scale structural ceramic precision machining formula comprise 57 parts by weight of mixture, 5 parts by weight of dispersing agent, 4 parts by weight of active agent, 8 parts by weight of bonding agent, 3 parts by weight of catalyst, 10 parts by weight of auxiliary agent, 9 parts by weight of grinding agent and 4 parts by weight of grinding material.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
A precision processing technique for large-scale structural ceramics,
the preparation process of the silicon nitride ceramic comprises the following steps:
s1: grinding, in order to fully react, grinding silicon carbide forming crystals and caking, wherein the product has low purity and large particles, and grinding liquid is added for post-treatment, so that the powder is crushed and ground, and the particles are more compact and uniform;
s2: adding composite abrasive, preparing silicon nitride powder into secondary granules with the granularity of about 0.1mm by using a cold isostatic pressing method, improving the pressing performance and flowability of the powder, wherein the cold isostatic pressing method is carried out in a closed environment, so that impurities can be prevented from being mixed into the powder, the integral quality after molding is damaged, and the cold isostatic pressing method is selected to complete granulation in order to ensure the purity of the powder and the quality after processing;
s3, the silicon nitride ceramic powder compounding technology generally adopts a liquid-powder phase mixing method, absolute ethyl alcohol is used as a dispersion medium, polyethylene glycol is used as a dispersion auxiliary agent, and ultrasonic waves are used for treating liquid phase call objects to finish mixing ingredients;
s4, adding the mixture, the binding agent and deionized water according to the proportion, granulating to improve the fluidity and the compressibility of the silicon nitride powder, and adding the powder after granulating the mixture into a metal cavity through dry-press forming and cold isostatic pressing to improve the strength;
s5, adding a dispersing agent to enable the particles to be ionized into ions and then to be adsorbed on the surfaces of the particles, forming an electric double layer structure on the surfaces of the particles, improving the surface charge density of the particles, overcoming the van der Waals attractive force among the particles through the effect of the same charge repulsive force on the surfaces, realizing the dispersing effect, enabling the high-purity silicon nitride powder to be a barren material, and ensuring that the formed spherical blank has enough strength and is formed by adding an active agent to change the characteristics of powder crystals, wherein the surface performance is very weak and the polymerization difficulty is high;
s6: the quality detection is carried out on the ball blank, the ball performance of the blank which is not finished in quality detection does not meet the processing standard, the blank is required to be sintered to strengthen the strength of the blank, after the sintering is finished, the ceramic ball blank is more compact, the density is increased, the strength is also increased along with the increase, and the preparation is made for the grinding processing of the ceramic ball;
s7: before preventing the decomposition of silicon nitride, embedding the blank ball into mixed powder of silicon nitride and boron nitride with the similar composition to that of the blank ball, wherein the mixed powder forms a gas phase balance environment on the surface of the ball blank to prevent the decomposition of silicon nitride;
s8: sintering process, temperature is controlled to beIn the range of 1700-2000 ℃, silicon nitride undergoes decomposition reaction at 1900 ℃ high temperature: si (Si) 3 N 4 ＝3Si+2N 2 In the sintering process, the process is carried out under certain nitrogen pressure, so that the silicon nitride is not decomposed, the nitrogen can prevent the decomposition of the silicon nitride and can also play a role in densification of density, and better blank quality is obtained;
s9: the auxiliary agent is added during the re-sintering, and the density after the re-sintering is more than 90 percent, even can reach 99 percent. And shrinkage is generally less than 6.5%.
The processing process of the silicon nitride ceramic comprises the following steps:
s1: the method comprises the steps of firing the formed silicon nitride ceramic balls, carrying out quality inspection and fluorescent flaw detection on blank balls, selecting extremely large balls and extremely small balls, carrying out rough grinding processing on the blank balls to remove 95% of the ceramic ball allowance, and ensuring that the processing allowance range of the blank balls is not excessively large and is within the range of 0.3-0.5mm so as to ensure that the processing can be carried out;
s2: after rough grinding and fine grinding, the granularity of the grinding material is 20-40 mu m, an oil agent or water agent grinding liquid is added, the rotating speed of a grinding plate is 48-120r/min, the pressure is 2-3Mpa, fine grinding is carried out, the ceramic ball has good appearance, but the surface of the processed ball is still rough, and the precision is lower;
s3: adding a compound abrasive, wherein the abrasive grain size is 1-3.5Mm, adding an oil or water agent grinding liquid, and performing preliminary grinding processing under the pressure of 1-2.5Mpa at the rotating speed of 25-60r/min, so as to improve the surface quality and processing precision of the ceramic balls and eliminate the stress on the surfaces of the ceramic balls;
s4: in the last step, compound abrasive is added, the granularity of the abrasive is less than 1 mu m, oil or water agent grinding liquid is added, the rotating speed of a grinding plate is 15-20r/min, the pressure is 1-3Mpa, the lapping processing is carried out, the grinding rotating speed is lower, the pressure cannot be too high, and the lapping steady state and the ball structure and the surface quality are not damaged;
s5: after lapping, the ceramic ball basically reaches the required precision, and finally polishing the ceramic ball to continuously improve the machining precision, and further improving the precision of the polished ball to finish the precision machining of the ceramic ball.
The embodiment is a control group, 57 parts of a preparation raw material mixture, 5 parts of a dispersing agent, 4 parts of an active agent, 8 parts of a binding agent, 3 parts of a catalyst, 10 parts of an auxiliary agent, 10 parts of an abrasive and 4 parts of an abrasive are in optimal proportion, the obtained ceramic ball blank has high performance, and the ceramic ball blank can achieve high strength, brittleness, stability and corrosion resistance after sintering.
Example 1
The precise machining recipe for large structural ceramic includes the materials including mixture 57 weight portions, dispersant 0 weight portions, active agent 4 weight portions, binding agent 8 weight portions, catalyst 3 weight portions, assistant 10 weight portions, and grinding agent 9 weight portions
And 4 parts of abrasive.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
Example 2
The precise machining recipe for large structural ceramic includes the materials including mixture 57 weight portions, dispersant 5 weight portions, active agent 0 weight portions, binding agent 8 weight portions, catalyst 3 weight portions, assistant 10 weight portions, and grinding agent 9 weight portions
And 4 parts of abrasive.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
Example 3
The precise machining recipe for large structural ceramic includes the materials including mixture 57 weight portions, dispersant 5 weight portions, active agent 4 weight portions, binding agent 0 weight portions, catalyst 3 weight portions, assistant 10 weight portions, and grinding agent 9 weight portions
And 4 parts of abrasive.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
Example 4
The precise machining recipe for large structural ceramic includes the materials including mixture 57 weight portions, dispersant 5 weight portions, active agent 4 weight portions, binding agent 8 weight portions, catalyst 3 weight portions, assistant 0 weight portions, and grinding agent 9 weight portions
And 4 parts of abrasive.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
Example 5
The precise machining recipe for large structural ceramic includes the materials including mixture 57 weight portions, dispersant 5 weight portions, active agent 3 weight portions, binding agent 7 weight portions, catalyst 3 weight portions, assistant 9 weight portions, and grinding agent 9 weight portions
And 4 parts of abrasive.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
Example 6
The precise machining recipe for large structural ceramic includes the materials including mixture 57 weight portions, dispersant 4 weight portions, active agent 4 weight portions, binding agent 8 weight portions, catalyst 3 weight portions, assistant 8 weight portions, and grinding agent 9 weight portions
And 4 parts of abrasive.
The mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
The dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
The active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane. The bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder. The catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
The auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following. The grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
The abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum, and is harder than silicon nitride ceramics.
The brittleness, strength, stability, and corrosion resistance of the ceramic ball bearings of examples 1-6 were determined by the following tests, brittleness: the brittleness is determined by chemical bond property and crystal structure, the material is difficult to relax stress by plastic deformation caused by sliding once in a stressed state, the existence of microcracks is easy to cause high concentration of stress, and then the microcracks are expanded to fracture, the brittleness a is influenced by grain size, cracks, porosity and cracks, a is less than or equal to 0.6 percent, the influence is judged, 0.6 percent is less than or equal to 3 percent, the brittleness is judged to be small, and a is more than 3 percent, and the brittleness is judged to be large.
Intensity: the strength b is affected by the porosity, grain size, grain thickness and shape, b is less than or equal to 15%, the strength is determined to be smaller, b is more than 15% and less than or equal to 33%, the strength is determined to be medium, and b is more than 33%, and the strength is determined to be larger. Stability: the ceramic material is characterized by having a capability of being subjected to abrupt change of external factors without breakage, wherein the stability c is less than or equal to 0.8%, the ceramic material is judged to be unstable, the stability c is more than 0.8% and less than or equal to 2.4%, and the stability c is more than 2.4%.
Corrosion resistance: the corrosion resistance d is less than or equal to 3.5%, the corrosion resistance d is judged to be not influenced, if 3.5% < d is less than or equal to 15%, the corrosion is judged to be mild, if 15% < d is less than or equal to 35%, the corrosion is judged to be moderate, and if d is more than 35%, the corrosion is judged to be heavy.
According to the invention, the comparison between the examples 1-4 and the comparison group shows that the dispersing agent has an influence on the brittleness of the ceramic ball blank body, the dispersing agent can be added appropriately to enable the ceramic ball blank body to be ionized into ions and then to be adsorbed on the surface of particles, so that the surface charge density of the ceramic ball blank body is improved, the Van der Waals attractive force among the particles is overcome through the effect of the same charge repulsive force on the surface, the forming rate and the forming strength of the ceramic ball blank body are improved by adding an appropriate amount of the active agent, the texture uniformity and the strength of the formed ball blank body are ensured, the stability of the ceramic ball blank body is influenced by adding an appropriate amount of the active agent, the internal structure of the ceramic ball blank body is more compact by adding an appropriate amount of the bonding agent, the corrosion resistance of the ceramic ball blank body is improved by adding an appropriate amount of the auxiliary agent, the corrosion resistance of the ceramic ball blank body is improved, the strength and the corrosion resistance of the ceramic ball blank body are also influenced by the active agent, the bonding agent and the auxiliary agent, and the influence on the brittleness and the corrosion resistance of the ceramic ball blank body are obtained by comparing the examples 5 and the examples 1-4.

Claims (10)

1. A large-scale structural ceramic precision machining formula is characterized in that: the preparation raw materials comprise, by weight, 47-65 parts of a mixture, 3-7 parts of a dispersing agent, 2-5 parts of an active agent, 6-9 parts of a binding agent, 1-5 parts of a catalyst, 7-13 parts of an auxiliary agent, 8-11 parts of an abrasive and 2-6 parts of an abrasive.
2. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the mixture is silicon dioxide (SiO 2 ) Carbon powder (C), silicon (S), nitrogen (N) 2 ) And SiO 2 -C mixture composition.
3. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the dispersing agent is one or more of absolute ethyl alcohol, polyethylene glycol, water glass, sodium humate, sodium hexametaphosphate, sodium tripolyphosphate, sodium citrate and ammonium salt.
4. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the active agent is one or more of CTAB, cyclohexane, octyl phenol polyoxyethylene ether and cyclohexane.
5. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the bonding agent is one or more of nitrogen, boron nitride, feldspar powder and low-melting borosilicate glass powder.
6. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the catalyst is Fe 2 O 3 、BaF 2 、CaF 2 One or more of the following.
7. According to claim 1The large-scale structural ceramic precision machining formula is characterized in that: the auxiliary agent is MgO, Y 2 O 3 、Al 2 O 3 、AlN、La 2 O 3 、TiO 2 、Mg 3 N 2 One or more of the following.
8. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the grinding agent is one or more of suspension, kerosene, oleic acid and engine oil, and the grinding liquid is a substance with strong adhesiveness.
9. The precision machining formula for large structural ceramics according to claim 1, wherein the formula comprises the following components: the abrasive is one or more of silicon carbide, chromium oxide, diamond and corundum.
10. A large-scale structural ceramic precision machining process is characterized in that:
the preparation process of the silicon nitride comprises the following steps:
s1: taking part of raw materials silicon dioxide and carbon powder, and carbonizing, reducing and nitriding SiO 2 The mixture with C powder enters N 2 And heating at 1200deg.C, wherein the reaction is performed in two steps, siO 2 Reducing under the action of C powder to generate Si;
s2: then Si and N are mixed at 1100-1500 DEG C 2 Reaction to produce Si 3 N 4 The general reaction formula is: 3SiO 2 +6C+2N 2 ＝Si 3 N 4 +6CO, sufficient carbon to ensure SiO is added to make the reaction more complete 2 Completely reacting;
s3: and SiO during the manufacturing process 2 Si is added into the mixed powder of-C 3 N 4 After 1300 ℃ heating treatment, the obtained silicon nitride powder crystal is different from the powder crystal obtained by simple carbonization and reduction, and the main shape of the crystal is sharp.
The preparation process of the silicon nitride ceramic comprises the following steps:
s1: grinding, in order to fully react, grinding silicon carbide forming crystals and caking, wherein the product has low purity and large particles, and grinding liquid is added for post-treatment, so that the powder is crushed and ground, and the particles are more compact and uniform;
s2: adding composite abrasive, preparing silicon nitride powder into secondary granules with the granularity of about 0.1mm by using a cold isostatic pressing method, improving the pressing performance and flowability of the powder, wherein the cold isostatic pressing method is carried out in a closed environment, so that impurities can be prevented from being mixed into the powder, the integral quality after molding is damaged, and the cold isostatic pressing method is selected to complete granulation in order to ensure the purity of the powder and the quality after processing;
s3, the silicon nitride ceramic powder compounding technology generally adopts a liquid-powder phase mixing method, absolute ethyl alcohol is used as a dispersion medium, polyethylene glycol is used as a dispersion auxiliary agent, and ultrasonic waves are used for treating liquid phase call objects to finish mixing ingredients;
s4, adding the mixture, the binding agent and deionized water according to the proportion, granulating to improve the fluidity and the compressibility of the silicon nitride powder, and adding the powder after granulating the mixture into a metal cavity through dry-press forming and cold isostatic pressing to improve the strength;
s5, adding a dispersing agent to enable the particles to be ionized into ions and then to be adsorbed on the surfaces of the particles, forming an electric double layer structure on the surfaces of the particles, improving the surface charge density of the particles, overcoming the van der Waals attractive force among the particles through the effect of the same charge repulsive force on the surfaces, realizing the dispersing effect, enabling the high-purity silicon nitride powder to be a barren material, and ensuring that the formed spherical blank has enough strength and is formed by adding an active agent to change the characteristics of powder crystals, wherein the surface performance is very weak and the polymerization difficulty is high;
s6: the quality detection is carried out on the ball blank, the ball performance of the blank which is not finished in quality detection does not meet the processing standard, the blank is required to be sintered to strengthen the strength of the blank, after the sintering is finished, the ceramic ball blank is more compact, the density is increased, the strength is also increased along with the increase, and the preparation is made for the grinding processing of the ceramic ball;
s7: before preventing the decomposition of silicon nitride, embedding the blank ball into mixed powder of silicon nitride and boron nitride with the similar composition to that of the blank ball, wherein the mixed powder forms a gas phase balance environment on the surface of the ball blank to prevent the decomposition of silicon nitride;
s8: in the sintering process, the temperature is controlled within the range of 1700-2000 ℃, and the silicon nitride can undergo decomposition reaction at the high temperature of 1900 ℃: si (Si) 3 N 4 ＝3Si+2N 2 In the sintering process, the process is carried out under certain nitrogen pressure, so that the silicon nitride is not decomposed, the nitrogen can prevent the decomposition of the silicon nitride and can also play a role in densification of density, and better blank quality is obtained;
s9: the auxiliary agent is added during the re-sintering, and the density after the re-sintering is more than 90 percent, even can reach 99 percent. And shrinkage is generally less than 6.5%.
The processing process of the silicon nitride ceramic comprises the following steps:
s1: the method comprises the steps of firing the formed silicon nitride ceramic balls, carrying out quality inspection and fluorescent flaw detection on blank balls, selecting extremely large balls and extremely small balls, carrying out rough grinding processing on the blank balls to remove 95% of the ceramic ball allowance, and ensuring that the processing allowance range of the blank balls is not excessively large and is within the range of 0.3-0.5mm so as to ensure that the processing can be carried out;
s2: after rough grinding and fine grinding, the granularity of the grinding material is 20-40 mu m, an oil agent or water agent grinding liquid is added, the rotating speed of a grinding plate is 48-120r/min, the pressure is 2-3Mpa, fine grinding is carried out, the ceramic ball has good appearance, but the surface of the processed ball is still rough, and the precision is lower;
s3: adding a compound abrasive, wherein the abrasive grain size is 1-3.5Mm, adding an oil or water agent grinding liquid, and performing preliminary grinding processing under the pressure of 1-2.5Mpa at the rotating speed of 25-60r/min, so as to improve the surface quality and processing precision of the ceramic balls and eliminate the stress on the surfaces of the ceramic balls;
s4: in the last step, compound abrasive is added, the granularity of the abrasive is less than 1 mu m, oil or water agent grinding liquid is added, the rotating speed of a grinding plate is 15-20r/min, the pressure is 1-3Mpa, the lapping processing is carried out, the grinding rotating speed is lower, the pressure cannot be too high, and the lapping steady state and the ball structure and the surface quality are not damaged;
s5: after lapping, the ceramic ball basically reaches the required precision, and finally polishing the ceramic ball to continuously improve the machining precision, and further improving the precision of the polished ball to finish the precision machining of the ceramic ball.
CN202310466991.1A 2023-04-26 2023-04-26 Precise machining process and formula for large-sized structural ceramic Withdrawn CN116477956A (en)

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