Low-temperature co-fired ceramic material and preparation method thereof
A low-temperature co-fired ceramic material comprises the following components in percentage by weight: 35-50% of CaO, 5-15% of B 2 O 3 , 40-55% of SiO 2 , 1-5% of nanometer Al 2 O 3 , 1-5% of MgO and 1-5% of nanometer ZrO 2 . A preparation method comprises the following steps: ball milling and mixing according to the formula, sintering at a high temperature, quenching in deionized water, grinding, performing wet ball-milling, drying and grinding; and finally, granulating to prepare a green body, discharging glue, and sintering, to obtain a low-temperature co-fired ceramic material. According to the low-temperature co-fired ceramic material and the preparation method thereof provided in the present disclosure, the prepared low-temperature co-fired ceramic material has the advantages of low dielectric constant, low loss, good overall performance and the like.
1. A method for preparing a low-temperature co-fired ceramic material, comprising the following steps:
S1: weighing the raw materials CaCO 3 , B 2 O 3 , SiO 2 , Al 2 O 3 , MgO, and ZrO 2 in percentage by weight: 35-50% of CaO, 5-15% of B 2 O 3 , 40-55% of SiO 2 , 1-5% of nanometer Al 2 O 3 , 1-5% of MgO and 1-5% of nanometer ZrO 2 , to obtain chemically pure CaO, B 2 O 3 , SiO 2 , nanometer Al 2 O 3 , MgO, nanometer ZrO 2 , ball milling and mixing mixed powder where ball milling medium is zirconia balls, and sieving through a 60-mesh screen after the mixed powder is mixed uniformly;
S2: sintering the sieved mixed powder obtained in Step S1 at a high temperature, and holding for a predetermined period of time, to melt and homogenize the mixed powder completely to obtain a melt;
S3: quenching the melt in deionized water, to obtain a transparent broken glass body;
S4: grinding the broken glass body, to obtain a fine glass body;
S5: performing wet ball milling on the fine glass body, drying, grinding, and sieving through a 120-mesh screen, to obtain a glass powder;
S6: granulating the glass powder with a granulation solution, sieving to obtain fine powder, and pressing the fine powder into a green body;
S7: discharging glue from the green body; and
S8: sintering the green body after glue discharge, to obtain the low-temperature co-fired ceramic material.
2. The preparation method according to claim 1 , wherein average particle size of the nanometer Al 2 O 3 is 60-100 nm, and the average particle size of the nanometer ZrO 2 is 80-100 nm.
3. The preparation method according to claim 1 , wherein the ball milling and mixing step in Step S1 is dry mixing for 4-8 h in a vibrational ball mill, and the weight ratio of the material to the balls in the ball milling and mixing step is 1:(2-4).
4. The preparation method according to claim 1 , wherein Step S2 comprises sintering at a high temperature of 1350-1500° C., and the holding time is 1-2.5 h.
5. The preparation method according to claim 1 , wherein in the wet ball milling step in Step S5, the weight ratio of material:ball:water is 1:4:1.5, the ball milling time is 6-10 h, and the rotational speed of the ball mill is 200-250 rpm.
6. The preparation method according to claim 1 , wherein the drying step in Step S5 takes place at 70-100° C., and the average particle size of the resulting glass powder is 0.5-2.0 μm.
7. The preparation method according to claim 1 , wherein Step S6 specifically comprises: adding a 10 wt % solution of polyvinyl alcohol in water to the glass powder, granulating, sieving the powder through a 60-mesh and a 200-mesh screen, and pressing the intermediate powder into a green body, where the press pressure is 220-260 MPa, and the press time is 10-20 s.
8. The preparation method according to claim 1 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.
9. The preparation method according to claim 2 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.
10. The preparation method according to claim 3 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.
11. The preparation method according to claim 4 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.
12. The preparation method according to claim 5 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.
13. The preparation method according to claim 6 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.
14. The preparation method according to claim 7 , wherein Step S7 specifically comprises: placing the green body in a muffle furnace, raising the temperature to 450-500° C. at a ramp rate of 0.5-1° C./min, and holding for 4-8 h, to discharge the organics; and Step S8 specifically comprises: placing the green body after glue discharge in a muffle furnace, sintering by raising the temperature to 840-880° C. at a ramp rate of 5-8° C./min, holding for 15-30 min, and then naturally cooling to room temperature with the furnace.