Agglomerated ceramic abrasive and method of making

Abstract

The present application relates to a kind of agglomerated ceramic abrasive, the raw material of the agglomerated ceramic abrasive, according to percentage by weight, including ceramic binder 25-30%, diamond micro powder 65-70%, titanium powder 1-3%, nitrate 2.5-5%, nickel sulfate 0.3-0.5%, aluminium zirconate 1-3%, after mixing uniformly with water, grinding;Then spray granulation, dry and sinter, i.e. the agglomerated ceramic abrasive is obtained.Compared with ordinary ceramic binder diamond agglomerated abrasive, the agglomerated ceramic abrasive prepared by the present application has the advantages of high hardness, uniform particle distribution, good grinding performance and the like.Sampling the agglomerated ceramic abrasive of the present application polishes marble tile, the surface of the tile does not appear relatively obvious scratch, surface consistency is good, and the polishing efficiency of marble tile is high.

Description

TECHNICAL FIELD

[0001] The present application relates to an agglomerated ceramic abrasive and a preparation method thereof, and belongs to the field of ceramic abrasives. BACKGROUND

[0002] The agglomerated ceramic abrasive is a new type of abrasive formed by bonding a large number of fine and irregular-shaped abrasives together to form a combined abrasive particle group with certain size, shape and strength through a special process. This abrasive has significant advantages in grinding processing, especially in improving grinding efficiency and reducing workpiece surface roughness. The agglomerated ceramic abrasive is mainly composed of three elements: abrasive, pore and binder. The abrasive is the main material for grinding processing; the binder is used to bond the fine abrasives together to form a large abrasive particle group with certain strength; and the pore has the function of temporarily storing grinding dust and coolant to prevent the grinding dust from remaining on the workpiece surface or the workpiece from being burned due to excessive grinding temperature. The agglomerated ceramic abrasive is widely used in the processing of silicon carbide and sapphire as well as semiconductors due to its excellent self-sharpening property, high temperature resistance, chemical corrosion resistance and ability to maintain stable cutting force of the grinding tool. Common preparation techniques for the agglomerated ceramic abrasive include mold pressing or casting forming and breaking method, rolling method, spray drying method, reverse microemulsion polymerization method and screen plate extrusion method. In the existing agglomerated ceramic abrasive, the ratio of the binder to the agglomerated ceramic abrasive is not reasonable, which leads to uneven coating of diamond particles, low holding force, and affects the service life of the abrasive. In addition, the size of the prepared ceramic abrasive particles is large, which leads to high surface roughness of the ground workpiece during the polishing process. SUMMARY

[0003] The present application provides an agglomerated ceramic abrasive and a preparation method thereof, which solves the problems of uneven coating of diamond particles, low holding force, and affects the service life of the abrasive in the existing agglomerated ceramic abrasive. In addition, the size of the prepared ceramic abrasive particles is large, which leads to high surface roughness of the ground workpiece during the polishing process.

[0004] To solve the above technical problems, the technical scheme adopted by the present application is as follows:

[0005] An agglomerated ceramic abrasive, the raw materials of the agglomerated ceramic abrasive include, in terms of weight percentage, 25-30% of ceramic binder, 65-70% of diamond micro powder, 1-3% of titanium powder, 2.5-5% of nitrate, 0.3-0.5% of nickel sulfate, and 1-3% of aluminum zirconate.

[0006] Further, preferably, the raw materials of the agglomerated ceramic abrasive include, in terms of weight percentage, 25% of ceramic binder, 65% of diamond micro powder, 3% of titanium powder, 5% of nitrate, 0.5% of nickel sulfate, and 1.5% of aluminum zirconate.

[0007] Further, preferably, the ceramic binder is composed of the following raw materials: Na2O 9%, silane coupling agent 0.5%, titanate coupling agent 0.5%, Al2O3 12%, B2O3 33%, SiO2 45%.

[0008] Further, preferably, the silane coupling agent is KH-550 or KH-560.

[0009] Further, preferably, the titanate coupling agent is TMC-301 or TMC-401.

[0010] Further, preferably, the preparation method of the ceramic binder is as follows:

[0011] (1) using pseudoboehmite as the aluminum source and 10% HNO3 as the peptizing agent, under the conditions of n(H+) / n(AlOOH) being 0.06, temperature being 50°C, and solid content being 10%, an aluminum sol is prepared;

[0012] (2) using tetraethyl orthosilicate as the silicon source and anhydrous ethanol as the peptizing agent, under the conditions of n(TEOS)∶n(EtOH)∶n(H2O)∶n(HNO3) being 1∶3.2∶6.5∶0.087, reaction temperature being 60°C, rotation speed being 200 r / min, and reaction time being 2 h, a silicon sol is prepared;

[0013] (3) boric acid and sodium nitrate are sequentially added to the aluminum sol and stirred to mix uniformly, then the silicon sol is added, and the solution is continuously heated to maintain the temperature at 70°C and the rotation speed at 200 r / min for 1 h to allow the substances in the solution to fully hydrolyze, then the silane coupling agent and the titanate coupling agent are added, and the rotation speed is 200 r / min for 30 min to mix uniformly;

[0014] (4) the mixed sol is aged at 100-120°C for 24-36 h, then is ball milled to pass through a 200-mesh screen, and the ceramic binder is prepared.

[0015] The preparation method of the agglomerated ceramic abrasive of the present application comprises the following steps:

[0016] (1) the ceramic binder, diamond micro-powder, titanium powder, molten salt, nickel sulfate, and aluminum zirconate are mixed in proportion, then water is added to make the solid content of the liquid 65-70%, and a ball mill or ultrasonic dispersion equipment is used to uniformly disperse the mixture to ensure uniform distribution of the components;

[0017] (2) spray granulation is performed; the spray pressure is 0.4-0.6 MPa, the air inlet temperature is 200-220°C, the outlet temperature is 100-110°C, and the spray hole diameter is 0.4-0.5 mm;

[0018] (3) after spray granulation, dry at 80-100℃ for 1h, then under nitrogen protection, heat to 500-550℃ at a heating rate of 2℃ / min, keep for 1.5-2h, heat to 650-700℃ at a heating rate of 5℃ / min, keep for 0.5-1h, and finally cool naturally;

[0019] (4) screen the cooled granules with a 180 mesh screen to obtain the agglomerated ceramic abrasive.

[0020] The present application has the following advantages:

[0021] The agglomerated ceramic abrasive of the present application uses ceramic binder, diamond micro powder, titanium powder, nitrate, nickel sulfate and aluminum zirconate as raw materials. Compared with the common ceramic binder diamond agglomerated abrasive, the agglomerated ceramic abrasive has the advantages of high hardness, uniform particle distribution and good grinding performance. The marble ceramic tile polished by the agglomerated ceramic abrasive of the present application has no obvious scratches on the surface and has good surface consistency, and the polishing efficiency of the marble ceramic tile is high. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all the other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0023] The pseudo-boehmite used in the present application has the following chemical composition (%): SiO2≤0.3%, Fe2O3≤0.03%, Na2O≤0.30, moisture≤20%, ignition loss≤24%, physicochemical performance peptization index: ≥95%, trihydrate≤5%, pore volume≥0.3mL / g, and specific surface area≥250m2 / g.

[0024] The diamond micro powder uses 180-200 mesh RVD diamond micro powder as the single particle abrasive of the agglomerated abrasive.

[0025] The ceramic binder used in the following embodiments of the present application is prepared by the above method.

[0026] Embodiment 1

[0027] An agglomerated ceramic abrasive, the raw materials of the agglomerated ceramic abrasive include, by weight percentage, ceramic binder 23%, diamond micro powder 70%, titanium powder 2%, nitrate 2.6%, nickel sulfate 0.4%, and aluminum zirconate 2%.

[0028] The ceramic binder is composed of the following raw materials: Na2O 9%, silane coupling agent 0.5%, titanate coupling agent 0.5%, Al2O3 12%, B2O3 33%, SiO2 45%.

[0029] The silane coupling agent is KH-560, and the titanate coupling agent is TMC-401. In this embodiment, TMC-401 is used.

[0030] The preparation method of the ceramic binder is as follows:

[0031] (1) using pseudoboehmite as the aluminum source and 10% HNO3 as the peptizing agent, an aluminum sol is prepared under the conditions of n(H + ) / n(AlOOH) 0.06, temperature 50°C, and solid content 10%;

[0032] (2) using tetraethyl orthosilicate as the silicon source and anhydrous ethanol as the peptizing agent, a silicon sol is prepared under the conditions of n(TEOS):n(EtOH):n(H2O):n(HNO3) = 1:3.2:6.5:0.087, reaction temperature 60°C, rotation speed 200 r / min, and time 2 h;

[0033] (3) boric acid and sodium nitrate are sequentially added to the aluminum sol and stirred to mix uniformly, then the silicon sol is added, and the solution is continuously heated to maintain the temperature at 70°C and the rotation speed at 200 r / min for 1 h to allow the substances in the solution to fully hydrolyze, then the silane coupling agent and the titanate coupling agent are added, and the mixture is stirred at the rotation speed of 200 r / min for 30 min to mix uniformly;

[0034] (4) the mixed sol is aged at 110°C for 24 h, then ball-milled through a 200-mesh screen to prepare the ceramic binder.

[0035] The preparation method of the agglomerated ceramic abrasive includes the following steps:

[0036] (1) the ceramic binder, diamond micro-powder, titanium powder, molten salt, nickel sulfate, and aluminum zirconate are mixed in proportion, then water is added to make the solid content of the liquid 65%, and a ball mill is used to uniformly disperse the mixture (ball milling conditions: corundum balls are added in the proportion of 1:1 of ball-to-material mass ratio, Φ50 mm and above account for 30%, and Φ50 mm and below account for 70%; rotation speed 60 r / min, and milling time 1 h) to ensure uniform distribution of the components;

[0037] (2) spray granulation is performed; the spray pressure is 0.4 MPa, the air inlet temperature is 210°C, the outlet temperature is 110°C, and the spray hole diameter is 0.5 mm;

[0038] (3) After spray granulation, dry at 100℃ for 1h, then under nitrogen protection, heat to 550℃ at a heating rate of 2℃ / min, keep for 2h, heat to 700℃ at a heating rate of 5℃ / min, keep for 0.5h, and finally cool naturally;

[0039] (4) Screen the cooled granules with a 180 mesh screen to obtain the agglomerated ceramic abrasive.

[0040] Examples 1-5 investigate the influence of different ceramic binder compositions on the agglomerated abrasive

[0041] The same as Example 1, except that the raw material ratio of the ceramic binder is different, as shown in Table 1.

[0042] The polishing performance and polishing efficiency of the obtained agglomerated abrasive are measured, and the specific method is as follows:

[0043] (1) Pile-up abrasive grinding and polishing performance:

[0044] The agglomerated abrasive prepared in different examples is used as the abrasive to configure the polishing liquid, and the specific composition of the polishing liquid is: agglomerated abrasive 5 parts, oleic acid 1 part, polyoxypropylene mannitol 1.5 parts, methyl cellulose 0.5 parts, fatty alcohol polyoxyethylene ether 0.5 parts, and water 91.5 parts.

[0045] A polishing tester is used to polish marble tiles, and the rotation speed is set to 150r / min and the polishing time is 5min. The surface morphology of the ground and polished marble tiles is observed; at the same time, the roughness of the polished workpiece surface is detected, and the specific results are shown in Table 1.

[0046] (2) Polishing liquid polishing efficiency:

[0047] The mass of the marble tile before and after polishing is measured, and the polishing efficiency of the polishing liquid on the marble tile is calculated by the following formula, and the specific results are shown in Table 1.

[0048] Polishing efficiency = (m1-m2) / m1*h.

[0049] Wherein: m1 and m2 are the mass before and after polishing, respectively, in g; h is the grinding time, in min.

[0050] Table 1 Experimental results of the influence of different ceramic binder compositions on the agglomerated abrasive

[0051]

[0052] As shown in Table 1, the agglomerated ceramic abrasive prepared in Example 1 has no obvious scratches on the polished marble tile surface, and the surface consistency is good, and the roughness is Ra 0.786 μm, and the polishing efficiency on the marble tile is 0.95 g / min. The agglomerated ceramic abrasive prepared in Comparative Examples 1-3 has more scratches on the marble tile surface, and the surface consistency is poor, and the roughness is Ra 1.079-1.125 μm, and the polishing efficiency on the marble tile is 0.68-0.71 g / min. It can be seen that the agglomerated ceramic abrasive of the present application has the silane coupling agent and the titanate coupling agent added in the ceramic binder, which can significantly improve the performance of the diamond agglomerated abrasive containing titanium powder. Compared with Comparative Example 1 without the silane coupling agent and the titanate coupling agent, the roughness is reduced by 30%, and the polishing efficiency is increased by 34%, and the improvement effect is obvious. The present application adds the silane coupling agent and the titanate coupling agent in the ceramic binder, the silane coupling agent mainly enhances the interface bonding through chemical bonding with inorganic and organic phases, and the titanate coupling agent further strengthens the bonding effect through interface activation and dispersion improvement. The two complement each other in the mechanism, and can more comprehensively improve the performance of the binder. The silanol group of the silane coupling agent and the titanium element of the titanate coupling agent can form a more complex chemical bond network with the inorganic phase in the ceramic binder, thereby significantly improving the mechanical strength and holding force of the binder. The joint action of the two coupling agents can optimize the interface structure between the ceramic binder and the diamond agglomerated abrasive, reduce the interface defects, and improve the uniformity and stability of the binder. Such ceramic binder can well coat the diamond particles, form uniform holding force, and the sol binder particle size is fine, which can make the agglomerated ceramic abrasive stable in the polishing process, and effectively reduce the surface roughness of the workpiece being polished.

[0053] Comparative Examples 6-9 investigate the influence of different raw material compositions on the agglomerated abrasive

[0054] The same as Example 1, except that the raw material ratio of the agglomerated abrasive is different, as shown in Table 2.

[0055] The polishing performance and polishing efficiency of the obtained agglomerated abrasive are determined, as shown in Table 2.

[0056] Table 2 Experimental results of the influence of different raw material compositions on the agglomerated abrasive

[0057]

[0058] As shown in Table 2, the agglomerated ceramic abrasive prepared in Example 1 has no obvious scratches on the polished marble tile surface, the surface uniformity is good, and the roughness is Ra 0.812 μm, and the polishing efficiency of the marble tile is 0.97 g / min. The agglomerated ceramic abrasive prepared in Comparative Example 6-93 has more scratches on the marble tile surface, the surface uniformity is poor, and the roughness is Ra 0.964-1.243 μm, and the polishing efficiency of the marble tile is 0.71-0.85 g / min. It can be seen that the performance of the agglomerated ceramic abrasive prepared in the present application is significantly better than that of Comparative Examples 6-9.

[0059] In the agglomerated abrasive prepared by compounding the ceramic binder and the diamond, titanium powder, nitrate, nickel sulfate and aluminum zirconate are added, and through the interaction of different mechanisms, the holding force of the diamond particles and the surface roughness of the abrasive are improved. Titanium powder reacts with the surface of diamond to form titanium carbide and form a strong chemical bond during high-temperature sintering, which significantly improves the interfacial bonding force between the ceramic binder and the diamond particles, thereby enhancing the holding force. Titanium powder improves the toughness of the ceramic binder through dispersion strengthening mechanism, reduces the fragmentation and shedding of the abrasive during use. Nitrate decomposes at high temperature to release oxygen and nitrogen, promotes the redox reaction in the sintering process, forms a uniform microstructure, improves the density and strength of the binder, and the gas generated by the decomposition of nitrate helps to reduce surface defects during sintering, thereby improving the surface roughness of the abrasive. Nickel sulfate as a sintering aid can reduce the sintering temperature of the ceramic binder, promote the densification of the binder, and improve its strength and hardness. Nickel sulfate reacts with titanium powder to form nickel-titanium alloy and other compounds, further enhancing the interfacial bonding force between the binder and the diamond particles. Aluminum zirconate is a high-melting-point ceramic material that can significantly improve the thermal stability and mechanical properties of the binder, ensuring the stability of the abrasive under high temperature and high pressure conditions. At the same time, the addition of aluminum zirconate can refine the grain size of the ceramic binder, reduce the surface roughness, and thus improve the surface quality of the abrasive.

[0060] Titanium powder and nickel sulfate synergistically enhance the interfacial bonding: titanium powder and nickel sulfate react to form nickel-titanium alloy and other compounds during sintering, further enhancing the interfacial bonding force between the binder and the diamond particles. The gas generated by the decomposition of nitrate and the sintering aid effect of nickel sulfate synergistically promote the uniform densification of the binder and improve the surface roughness. The thermal stability and mechanical properties of aluminum zirconate combined with the interfacial enhancement of titanium powder and nickel sulfate significantly improve the overall performance of the abrasive.

[0061] Titanium powder, nitrate, nickel sulfate and aluminum zirconate have their own characteristics and synergistic effects, making the abrasive have higher diamond particle holding force and lower surface roughness, thereby improving the overall performance and service life of the abrasive.

[0062] Example 2

[0063] An agglomerated ceramic abrasive, raw materials of the agglomerated ceramic abrasive comprising, in percentage by weight, ceramic binder 25%, diamond micro-powder 65%, titanium powder 3%, nitrate 5%, nickel sulfate 0.5%, aluminum zirconate 1.5%,

[0064] The ceramic binder is composed of the following raw materials: Na2O 9%, silane coupling agent 0.5%, titanate coupling agent 0.5%, Al2O3 12%, B2O3 33%, SiO2 45%.

[0065] The silane coupling agent is KH-550, and the titanate coupling agent is TMC-301.

[0066] The preparation method is as follows:

[0067] (1) taking pseudo-boehmite as aluminum source and 10% HNO3 as peptizing agent, an aluminum sol is prepared under the conditions of n(H + ) / n(AlOOH) 0.06, temperature 50°C, and solid content 10%;

[0068] (2) taking tetraethyl orthosilicate as silicon source and anhydrous ethanol as peptizing agent, a silicon sol is prepared under the conditions of n(TEOS)∶n(EtOH)∶n(H2O)∶n(HNO3) = 1∶3.2∶6.5∶0.087, reaction temperature 60°C, rotation speed 200 r / min, and reaction time 2 h;

[0069] (3) boric acid and sodium nitrate are sequentially added to the aluminum sol and stirred to mix uniformly, then the silicon sol is added, and the solution is continuously heated to maintain the temperature at 70°C, the rotation speed is 200 r / min, and the solution is stirred for 1 h to make the substances in the solution fully hydrolyze, then the silane coupling agent and the titanate coupling agent are added, the rotation speed is 200 r / min, and the mixture is stirred for 30 min to mix uniformly;

[0070] (4) the mixed sol is aged at 100°C for 36 h, then is ball milled through a 200-mesh screen to obtain the ceramic binder.

[0071] The preparation method comprises the following steps:

[0072] (1) the ceramic binder, diamond micro-powder, titanium powder, fused salt, nickel sulfate, and aluminum zirconate are mixed in proportion, then water is added to make the solid content of the liquid 65%, and a ball mill is used to uniformly disperse the mixture and ensure uniform distribution of the components;

[0073] (2) spray granulation is performed; the spray pressure is 0.5 MPa, the air inlet temperature is 220°C, the outlet temperature is 110°C, and the spray hole diameter is 0.5 mm;

[0074] (3) After the spray granulation, dry at 100℃ for 1h, then under the protection of nitrogen, heat to 550℃ at a heating rate of 2℃ / min, keep for 2h, heat to 650℃ at a heating rate of 5℃ / min, keep for 0.5h, and finally cool naturally;

[0075] (4) Screen the cooled granules with a 180-mesh screen to obtain the agglomerated ceramic abrasive.

[0076] The agglomerated ceramic abrasive prepared has no obvious scratches on the surface of the polished marble tile, has good surface consistency, and has a roughness of Ra 0.678 μm. The polishing efficiency for the marble tile is calculated to be 1.08 g / min.

[0077] Example 3

[0078] An agglomerated ceramic abrasive, wherein the raw materials of the agglomerated ceramic abrasive comprise, by weight percentage, ceramic binder 25%, diamond micro-powder 65%, titanium powder 3%, nitrate 3.7%, nickel sulfate 0.3%, aluminum zirconate 3%, and

[0079] The ceramic binder is composed of the following raw materials: Na2O 9%, silane coupling agent 0.5%, titanate coupling agent 0.5%, Al2O3 12%, B2O3 33%, and SiO2 45%.

[0080] The silane coupling agent is KH-550 or KH-560, and KH-560 is used in this example. The titanate coupling agent is TMC-301 or TMC-401, and TMC-401 is used in this example.

[0081] The preparation method is as follows:

[0082] (1) Using pseudoboehmite as the aluminum source and 10% HNO3 as the peptizing agent, an aluminum sol is prepared under the conditions of n(H2O)∶n(AlOOH) 0.06, temperature 50℃, and solid content 10%; +

[0083] (2) Using tetraethyl orthosilicate as the silicon source and anhydrous ethanol as the peptizing agent, a silicon sol is prepared under the conditions of n(TEOS)∶n(EtOH)∶n(H2O)∶n(HNO3) 1∶3.2∶6.5∶0.087, reaction temperature 60℃, rotation speed 200 r / min, and reaction time 2h.

[0084] ​(3) the boric acid and sodium nitrate are added into the aluminum sol in sequence, stirred and mixed uniformly, then the silica sol is added, the heating is continued, the temperature is kept at 70℃, the rotating speed is 200r / min, the solution is stirred for 1 hour to make the substances in the solution hydrolyze sufficiently, then the silane coupling agent and the titanate coupling agent are added, the rotating speed is 200r / min, the mixture is stirred for 30 minutes to be mixed uniformly;

[0085] (4) the mixed sol is aged at 120℃ for 24 hours, then is ball milled through a 200 mesh screen to obtain the ceramic bond.

[0086] The preparation method comprises the following steps:

[0087] (1) the ceramic bond, the diamond micro powder, the titanium powder, the molten salt, the nickel sulfate and the aluminum zirconate are mixed in proportion, then water is added to make the solid content of the liquid 65%, the ball mill is used to uniformly disperse the mixture and ensure the uniform distribution of the components;

[0088] (2) the spray granulation is carried out; the spray pressure is 0.6MPa, the air inlet temperature is 200℃, the outlet temperature is 100℃, the spray hole diameter is 0.4mm;

[0089] (3) after the spray granulation, the mixture is dried at 100℃ for 1 hour, then is heated to 500℃ at a heating speed of 2℃ / min under nitrogen protection, is kept for 2 hours, is heated to 700℃ at a heating speed of 5℃ / min, is kept for 0.5 hour, and finally is naturally cooled;

[0090] (4) the granules after cooling are sieved by using a 180 mesh screen to obtain the agglomerated ceramic abrasive.

[0091] After the agglomerated ceramic abrasive is used to polish the marble ceramic tile, no obvious scratches appear on the surface of the ceramic tile, the surface consistency is good, the roughness is Ra0.906μm, and the polishing efficiency of the marble ceramic tile is 0.95g / min.

[0092] Example 4

[0093] An agglomerated ceramic abrasive, the raw materials of the agglomerated ceramic abrasive comprise, in percentage by weight, the ceramic bond 30%, the diamond micro powder 65%, the titanium powder 1%, the nitrate 2.5%, the nickel sulfate 0.5%, the aluminum zirconate 1%.

[0094] The ceramic bond is composed of the following raw materials: Na2O 9%, the silane coupling agent 0.5%, the titanate coupling agent 0.5%, Al2O3 12%, B2O3 33%, SiO2 45%.

[0095] The silane coupling agent is KH-550 or KH-560, and the titanium coupling agent is TMC-301 or TMC-401. In this embodiment, KH-560 and TMC-401 are used.

[0096] The preparation method is as follows:

[0097] (1) Using pseudoboehmite as the aluminum source and 10% HNO3 as the peptizing agent, an aluminum sol is prepared under the conditions of n(H + ) / n(AlOOH) of 0.06, a temperature of 50°C, and a solid content of 10%;

[0098] (2) Using tetraethyl orthosilicate as the silicon source and anhydrous ethanol as the peptizing agent, a silicon sol is prepared under the conditions of n(TEOS)∶n(EtOH)∶n(H2O)∶n(HNO3) of 1∶3.2∶6.5∶0.087, a reaction temperature of 60°C, a rotation speed of 200 r / min, and a reaction time of 2 h;

[0099] (3) Boric acid and sodium nitrate are sequentially added to the aluminum sol, which is stirred and mixed uniformly, and then the silicon sol is added. The solution is continuously heated to maintain a temperature of 70°C and a rotation speed of 200 r / min for 1 h to allow the substances in the solution to fully hydrolyze. Then, the silane coupling agent and the titanium coupling agent are added, and the mixture is stirred at a rotation speed of 200 r / min for 30 min to achieve uniform mixing;

[0100] (4) The mixed sol is aged at 110°C for 24 h, and then ball-milled through a 200-mesh screen to obtain the ceramic binder.

[0101] The preparation method comprises the following steps:

[0102] (1) The ceramic binder, diamond micro-powder, titanium powder, molten salt, nickel sulfate, and aluminum zirconate are mixed in proportion, and then water is added to make the solid content of the liquid 70%. A ball mill is used to uniformly disperse the mixture and ensure uniform distribution of the components;

[0103] (2) Spray granulation is performed at a spray pressure of 0.4 MPa, an air inlet temperature of 210°C, an outlet temperature of 110°C, and a spray hole diameter of 0.5 mm;

[0104] (3) After spray granulation, the mixture is dried at 100°C for 1 h, and then heated to 550°C at a temperature rising speed of 2°C / min under nitrogen protection, maintained for 2 h, heated to 650°C at a temperature rising speed of 5°C / min, maintained for 0.5 h, and finally naturally cooled;

[0105] (4) The cooled granules are sieved through a 180-mesh screen to obtain the agglomerated ceramic abrasive.

[0106] The prepared agglomerated ceramic abrasive has no obvious scratch on the surface of polished marble tile, has good surface consistency, and has a roughness of Ra 0.785 μm, and a polishing efficiency of 0.93 g / min for marble tile.

[0107] Example 5

[0108] An agglomerated ceramic abrasive, raw materials of the agglomerated ceramic abrasive include, by weight percentage, ceramic binder 26%, diamond micro-powder 66%, titanium powder 2%, nitrate 3.2%, nickel sulfate 0.3%, aluminum zirconate 2.5%, and

[0109] The ceramic binder is composed of the following raw materials: Na2O 9%, silane coupling agent 0.5%, titanate coupling agent 0.5%, Al2O3 12%, B2O3 33%, and SiO2 45%.

[0110] The silane coupling agent is KH-550 or KH-560, and the titanate coupling agent is TMC-301 or TMC-401, and KH-560 and TMC-401 are used in this example.

[0111] The preparation method is as follows:

[0112] (1) using pseudo-boehmite as aluminum source and 10% HNO3 as peptizing agent, an aluminum sol is prepared under the conditions of n(H2O)∶n(AlOOH) 0.06, temperature 50°C, and solid content 10%; +

[0113] (2) using tetraethyl orthosilicate as silicon source and anhydrous ethanol as peptizing agent, a silicon sol is prepared under the conditions of n(TEOS)∶n(EtOH)∶n(H2O)∶n(HNO3) 1∶3.2∶6.5∶0.087, reaction temperature 60°C, rotation speed 200 r / min, and reaction time 2 h;

[0114] (3) boric acid and sodium nitrate are sequentially added to the aluminum sol and stirred to mix uniformly, then the silicon sol is added, and the solution is continuously heated to maintain the temperature at 70°C, and stirred at a rotation speed of 200 r / min for 1 h to make the substances in the solution fully hydrolyze, then the silane coupling agent and the titanate coupling agent are added, and stirred at a rotation speed of 200 r / min for 30 min to mix uniformly;

[0115] (4) the mixed sol is aged at 100°C for 36 h, then ball-milled through a 200-mesh screen to obtain the ceramic binder.

[0116] The preparation method includes the following steps:

[0117] ​(1) ceramic binder, diamond powder, titanium powder, molten salt, nickel sulfate and aluminum zirconate are mixed in proportion, then water is added to make the solid content of the liquid 65-70%, a ball mill is used to uniformly disperse the mixture and ensure uniform distribution of each component;

[0118] (2) spray granulation; the spray pressure is 0.4 MPa, the air inlet temperature is 210℃, the outlet temperature is 110℃, and the spray hole diameter is 0.5 mm;

[0119] (3) after spray granulation, drying at 100℃ for 1h, then under nitrogen protection, heating to 550℃ at a heating rate of 2℃ / min, holding for 1.5h, heating to 650℃ at a heating rate of 5℃ / min, holding for 0.5h, and finally natural cooling;

[0120] (4) the cooled granules are sieved with a 180 mesh screen, and the agglomerated ceramic abrasive is obtained.

[0121] The prepared agglomerated ceramic abrasive has no obvious scratches on the surface of the polished marble ceramic tile, the surface consistency is good, the roughness is Ra0.801μm, and the polishing efficiency of the marble ceramic tile is 0.93g / min.

[0122] The above only describes the preferred embodiments of the present application and is not intended to limit the present application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. An agglomerated ceramic abrasive characterized by: The raw material of the agglomerated ceramic abrasive comprises, in percentage by weight, 25-30% of ceramic binder, 65-70% of diamond micro powder, 1-3% of titanium powder, 2.5-5% of nitrate, 0.3-0.5% of nickel sulfate, and 1-3% of aluminum zirconate, wherein the ceramic binder is composed of 9% of Na2O, 0.5% of silane coupling agent, 0.5% of titanate coupling agent, 12% of Al2O3, 33% of B2O3, and 45% of SiO2. The preparation method of the ceramic binder is as follows: (1) with pseudo-boehmite as aluminum source and 10% HNO3 as peptizing agent, an aluminum sol was prepared under the conditions of n(HNO3) / n(AlOOH) 0.06, temperature 50 ℃ and solid content 10%; + ) / n( AlOOH) as 0.06, temperature as 50 ℃ and solid content as 10%. (2) under the conditions of n(TEOS):n(EtOH):n(H2O):n(HNO3)=1:3.2:6.5:0.087, a reaction temperature of 60°C, a rotation speed of 200 r / min, and a reaction time of 2 h, a silica sol is prepared by using tetraethyl orthosilicate as a silicon source and anhydrous ethanol as a peptizing agent; (3) boric acid and sodium nitrate are sequentially added to the aluminum sol and stirred to be uniformly mixed, then the silica sol is added, and the solution is continuously heated at a temperature of 70°C and a rotation speed of 200 r / min for 1 h to make the substances in the solution fully hydrolyze, then the silane coupling agent and the titanate coupling agent are added, and stirred at a rotation speed of 200 r / min for 30 min to be uniformly mixed; (4) the mixed sol is aged at 100-120°C for 24-36 h, and then ball-milled through a 200-mesh screen to obtain the ceramic binder.

2. The agglomerated ceramic abrasive according to claim 1, wherein: The raw material of the agglomerated ceramic abrasive comprises, in percentage by weight, 25-30% of ceramic binder, 65-70% of diamond micro powder, 1-3% of titanium powder, 2.5-5% of nitrate, 0.3-0.5% of nickel sulfate, and 1-3% of aluminum zirconate, wherein the ceramic binder is composed of 9% of Na2O, 0.5% of silane coupling agent, 0.5% of titanate coupling agent, 12% of Al2O3, 33% of B2O3, and 45% of SiO2.

3. The agglomerated ceramic abrasive according to claim 1, wherein: The silane coupling agent is KH-550 or KH-560.

4. The agglomerated ceramic abrasive according to claim 1, wherein: The titanate coupling agent is TMC-301 or TMC-401.

5. The method of producing agglomerated ceramic abrasive according to any one of claims 1 to 4, characterized in that: The method comprises the following steps: (1) the ceramic binder, the diamond micro powder, the titanium powder, the nitrate, the nickel sulfate, and the aluminum zirconate are mixed in proportion, then water is added to make the solid content of the liquid 65-70%, and a ball mill or an ultrasonic dispersion device is used to uniformly disperse the mixture to ensure uniform distribution of the components; (2) spray granulation is performed, the spray pressure is 0.4-0.6 MPa, the air inlet temperature is 200-220°C, the outlet temperature is 100-110°C, and the spray hole diameter is 0.4-0.5 mm; (3) after the spray granulation, the granules are dried at 80-100°C for 1 h, then heated to 500-550°C at a temperature rising speed of 2°C / min under nitrogen protection, kept at the temperature for 1.5-2 h, heated to 650-700°C at a temperature rising speed of 5°C / min, kept at the temperature for 0.5-1 h, and finally naturally cooled; (4) the cooled granules are sieved through a 180-mesh screen to remove large particles, and the agglomerated ceramic abrasive is obtained.

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