CN112299847A - 5G communication signal-based unshielded microcrystalline ceramic backboard preparation method - Google Patents
5G communication signal-based unshielded microcrystalline ceramic backboard preparation method Download PDFInfo
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Abstract
The invention discloses a preparation method of a 5G communication signal based unshielded microcrystalline ceramic backboard, which is used for respectively weighing high-purity Y2O3Powder, high purity Gd2O3Powder and high-purity ZrO2The powder is used as raw material powder, dispersant, plasticizer and binder are added for ball milling and mixing; directly carrying out tape casting molding after filtering, carrying out custom cutting and stacking on the obtained biscuit, carrying out warm isostatic pressing on the obtained biscuit, shaping, and then carrying out degreasing; vacuum sintering the degreased blank, naturally cooling to room temperature, adding into liquid nitrogen, storing for a period of time, taking out the ceramic from the liquid nitrogen, directly placing into a vacuum sintering furnace, sintering again, naturally coolingAnd cooling to room temperature, and annealing to obtain the microcrystalline ceramic backboard. The microcrystalline ceramic backboard prepared by the invention has excellent performance, no shielding on 5G communication signals, good jade texture and luster after polishing, low preparation cost and simple preparation process.
Description
Technical Field
The invention relates to the technical field of ceramic backboard preparation, in particular to a method for preparing a 5G communication signal-based unshielded microcrystalline ceramic backboard.
Background
With the huge breakthrough of science and technology, the internet of things industry is rapidly developed; mobile communication networks have also evolved from 2G, 3G to 4G, changing people's lives step by step. Nowadays, 5G signal base stations are becoming popular, which marks the arrival of the world of everything interconnection, which means that intelligent products based on 5G communication networks have become the mainstream of the market. At present, various manufacturers of large electronic products have released their own electronic products based on the 5G communication network.
However, the 5G communication network based on the millimeter wave (MMW) data transmission means has key technical problems of unstable transmission signal, short transmission distance, small coverage range and the like. Although the layout strategy of the micro base station can solve the partial problems existing in the 5G communication network, the signal shielding problem existing in the intelligent product cannot be effectively processed. The fundamental reason for the phenomenon is that the metal material has obvious absorption on the 5G high-frequency antenna, so that the finding and preparation of the backboard material without shielding on the 5G transmission signal have great commercial application value.
Among various materials existing in the market, glass and ceramic are widely applied to various intelligent products due to the advantage that the glass and the ceramic do not shield 5G signals. However, glass has poor wear resistance and low thermal conductivity, so that the glass cannot be an ideal backboard material for 5G intelligent products.
Chinese patent application CN104961461A discloses a preparation method of a zirconia ceramic mobile phone backboard, which prepares the zirconia ceramic mobile phone backboard by doping modification means of yttria-stabilized zirconia powder and combining a film tape casting technology. However, the preparation materials used in the method are toluene and isopropanol, which have great harm to the environment.
The Chinese patent application CN106187170A uses a dry pressing method to dry-press and mold the zirconia granulated powder, then packages the zirconia granulated powder, puts the packaged blank into an isostatic press for isostatic pressing, then puts the blank into a kiln to sinter into a ceramic piece, then puts the ceramic piece into a re-leveling kiln for re-sintering, and finally obtains the zirconia ceramic mobile phone backboard product after the working procedures of grinding, cutting, fine grinding and polishing. However, this method requires multiple pressing and does not achieve net shape forming of the back sheet material.
Disclosure of Invention
The invention aims to provide a preparation method of a 5G communication signal-based unshielded microcrystalline ceramic backboard, which has an environment-friendly preparation process and is easy to form.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a 5G communication signal based unshielded microcrystalline ceramic backboard comprises the following specific steps:
(1) separately weigh high purity Y2O3Powder, high purity Gd2O3Powder and high-purity ZrO2Adding the powder into a ball milling tank, wherein Y is2O3The addition amount is Y2O3With Gd2O30.1-0.9 wt.% of the mixed powder, ZrO 22The addition amount is Y2O3With Gd2O30.1-2 wt.% of the mass of the mixed powder;
(2) adding a dispersing agent and a solvent into the mixed powder obtained in the step (1) for ball milling, wherein the ball milling rotation speed is 80-300 r/min, the ball milling time is 15-36 h, and the solid content of the slurry is adjusted to be 45-55 wt%; the adding amount of the dispersing agent is 0.4-1.5 wt% of the total mass of the mixed raw material powder;
(3) sequentially adding a plasticizer and a binder into the slurry obtained in the step (2), wherein the addition amount of the plasticizer is 5-10 wt% of the total mass of the mixed raw material powder, and the addition amount of the binder is 5-10 wt% of the total mass of the mixed raw material powder, and continuing ball milling for 16-36 hours;
(4) filtering the slurry obtained in the step (3), and then directly carrying out tape casting to obtain a ceramic biscuit;
(5) carrying out custom cutting and stacking on the biscuit obtained in the step (4), carrying out warm isostatic pressing on the obtained biscuit, shaping the edge of the biscuit, and then degreasing;
(6) vacuum sintering the degreased blank in the step (5), wherein the sintering temperature is 1200-1500 ℃, the temperature is kept for 1-5 h, the ceramic is taken out, naturally cooled to room temperature, added into liquid nitrogen, and stored in the liquid nitrogen for 1-3 h;
(7) taking out the ceramic from the liquid nitrogen, directly putting the ceramic into a vacuum sintering furnace, heating to 1200-1500 ℃ at a speed of 10-30 ℃/min, heating to 1750-1930 ℃ at a speed of 1-5 ℃/min, preserving heat for 2-10 h, taking out the ceramic, naturally cooling to room temperature, annealing at an annealing temperature of 1100-1500 ℃ for 10-20 h, and naturally cooling to room temperature to obtain the 5G communication signal-based unshielded microcrystalline ceramic backboard.
Preferably, the ball milling in the step (2) is roller ball milling, the material of the milling ball is zirconia, and the diameter of the milling ball is 20-80 mm.
Preferably, the dispersant in the step (2) is one or more of NP-10, herring oil and castor oil; the solvent is a mixed solution of butanone and absolute ethyl alcohol, and the mass ratio of the butanone to the absolute ethyl alcohol is 0.5-0.8.
Preferably, the plasticizer in step (3) is one or more of butyl benzyl phthalate, dibutyl phthalate and propylene carbonate.
Preferably, the binder in step (3) is one or more of polyvinyl butyral, ethyl methacrylate and polyacrylic acid.
Preferably, the specific parameters of the tape casting process in the step (4) are as follows: the first section drying temperature of the casting machine is 25-35 ℃, the second section drying temperature is 30-40 ℃, and the casting speed is 10-50 cm/min, so that the casting biscuit with a smooth, defect-free, flat and uniform surface can be obtained.
Preferably, the temperature of the liquid nitrogen in the step (6) is 213-263K.
Compared with the prior art, the invention has the following beneficial effects:
1. the microcrystalline ceramic back plate prepared by the invention has excellent mechanical impact resistance, temperature shock resistance and electron corrosion resistance, and is low in preparation cost and simple in preparation process.
2. The microcrystalline ceramic back plate prepared by the invention has no shielding effect on 5G communication signals, and can be used for preparing a ceramic rear cover of a mobile phone.
3. The microcrystal ceramic back plate prepared by the invention has good jade texture and luster after being polished.
Drawings
FIG. 1 is a pictorial representation of a sample of polished microcrystalline ceramic having a diameter of about 65mm as prepared in example 1.
FIG. 2 is an SEM image of a ceramic sample prepared in example 1.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
A preparation method of a 5G communication signal based unshielded microcrystalline ceramic backboard comprises the following specific steps:
(1) separately weigh high purity Y2O3Powder, high purity Gd2O3Powder and high-purity ZrO2Adding the powder into a nylon ball milling tank, wherein Y is2O3The addition amount is Y2O3With Gd2O30.9 wt.% of the mixed powder mass, ZrO2The addition amount is Y2O3With Gd2O31 wt.% of the mass of the mixed powder;
(2) adding a dispersant NP-10 and a solvent into the mixed powder obtained in the step (1) to perform roller ball milling, wherein the grinding ball is made of zirconia, the diameter of the grinding ball is 30mm, the ball milling speed is 200r/min, the ball milling time is 20 hours, and the solid content of the slurry is adjusted to 52 wt.%; the adding amount of the dispersing agent is 1 wt% of the total mass of the mixed raw material powder, and the solvent is a mixed solution of butanone and absolute ethyl alcohol (the mass ratio of the butanone to the absolute ethyl alcohol is 0.5);
(3) sequentially adding a plasticizer butyl benzyl phthalate and a binder polyvinyl butyral into the slurry obtained in the step (2), wherein the addition amount of the plasticizer is 6 wt% of the total mass of the mixed raw material powder, and the addition amount of the binder is 6 wt% of the total mass of the mixed raw material powder, and continuing ball milling for 24 hours;
(4) filtering the slurry obtained in the step (3), and directly carrying out tape casting molding, wherein the first-stage drying temperature of the tape casting machine is 30 ℃, the second-stage drying temperature is 35 ℃, and the tape casting speed is 40cm/min, so as to obtain a ceramic biscuit;
(5) cutting the biscuit obtained in the step (4) into a wafer with the diameter of 78mm, stacking the wafer with the number of stacked layers of 57, carrying out warm isostatic pressing on the obtained biscuit, cutting and shaping the edge of the biscuit in a laser cutting mode, and then degreasing;
(6) vacuum sintering the degreased blank in the step (5), keeping the sintering temperature at 1300 ℃, preserving the heat for 1h, taking out the ceramic, naturally cooling to room temperature, adding the ceramic into liquid nitrogen at 248K, and preserving the ceramic in the liquid nitrogen for 2 h;
(7) taking out the ceramic from the liquid nitrogen, directly putting the ceramic into a vacuum sintering furnace, heating to 1300 ℃ at a speed of 20 ℃/min, heating to 1780 ℃ at a speed of 2 ℃/min, preserving heat for 6h, taking out the ceramic, naturally cooling to room temperature, annealing at the annealing temperature of 1200 ℃ for 15h, and naturally cooling to room temperature to obtain the 5G communication signal-based unshielded microcrystalline ceramic backboard.
FIG. 1 is a schematic diagram of a polished microcrystalline ceramic sample having a diameter of about 65mm prepared in example 1, and it can be seen from the schematic diagram that the surface of the sample is glossy and has a good jade texture.
The SEM image of the ceramic sample prepared in example 1 shown in FIG. 2 shows that the crystallite ceramic sample has a grain size of less than 10 μm.
Table 1 shows the experimental test result that the 5G mobile phone test signal passes through the ceramic backplate with the thickness of 8mm, and the 5G signal test confirms that the microcrystalline ceramic backplate prepared in this embodiment has no shielding for the 5G communication signal.
TABLE 15G Signal test results
| Network name/signal type | Signal strength (without shielding) | Signal strength (with ceramic shield) |
| China telecom/SA | 107dBm 33asu | 107dBm 33asu |
| China Mobile/NSA | 122dBm 33asu | 122dBm 33asu |
Example 2
A preparation method of a 5G communication signal based unshielded microcrystalline ceramic backboard comprises the following specific steps:
(1) separately weigh high purity Y2O3Powder, high purity Gd2O3Powder and high-purity ZrO2Adding the powder into a nylon ball milling tank, wherein Y is2O3The addition amount is Y2O3With Gd2O30.1 wt% of the total mass of the mixed powder, ZrO2The addition amount is Y2O3With Gd2O32 wt.% of the total mass of the mixed powder;
(2) adding dispersing agent herring oil and solvent into the mixed powder obtained in the step (1) to perform roller ball milling, wherein the grinding balls are made of zirconia, the diameter of the grinding balls is 50mm, the ball milling speed is 80r/min, the ball milling time is 36h, and the solid content of the slurry is adjusted to 45 wt.%; the addition amount of the dispersing agent is 0.4 wt% of the total mass of the mixed raw material powder, and the solvent is a mixed solution of butanone and absolute ethyl alcohol (the mass ratio of the butanone to the absolute ethyl alcohol is 0.6);
(3) sequentially adding a plasticizer dibutyl phthalate and a binder ethyl methacrylate into the slurry obtained in the step (2), wherein the adding amount of the plasticizer is 5 wt% of the total mass of the mixed raw material powder, and the adding amount of the binder is 5 wt% of the total mass of the mixed raw material powder, and continuing ball milling for 16 hours;
(4) filtering the slurry obtained in the step (3), and directly carrying out tape casting molding, wherein the first-stage drying temperature of the tape casting machine is 25 ℃, the second-stage drying temperature is 30 ℃, and the tape casting speed is 10cm/min, so as to obtain a ceramic biscuit;
(5) cutting the biscuit obtained in the step (4) into a wafer with the diameter of 78mm, stacking the wafer with 65 layers, carrying out warm isostatic pressing on the obtained biscuit, cutting and shaping the edge of the biscuit in a laser cutting mode, and degreasing;
(6) vacuum sintering the degreased blank in the step (5), keeping the sintering temperature at 1200 ℃, keeping the temperature for 1h, taking out the ceramic, naturally cooling to room temperature, adding the ceramic into 213K liquid nitrogen, and preserving in the liquid nitrogen for 1 h;
(7) taking out the ceramic from the liquid nitrogen, directly putting the ceramic into a vacuum sintering furnace, heating to 1200 ℃ at a speed of 10 ℃/min, heating to 1750 ℃ at a speed of 1 ℃/min, preserving heat for 2h, taking out the ceramic, naturally cooling to room temperature, annealing at an annealing temperature of 1100 ℃ for 20h, and naturally cooling to room temperature to obtain the 5G communication signal-based unshielded microcrystalline ceramic backboard.
The 5G signal test confirms that the microcrystalline ceramic backboard prepared in the embodiment has no shielding to 5G communication signals.
Example 3
A preparation method of a 5G communication signal based unshielded microcrystalline ceramic backboard comprises the following specific steps:
(1) separately weigh high purity Y2O3Powder, high purity Gd2O3Powder and high-purity ZrO2Adding the powder into a nylon ball milling tank, wherein Y is2O3The addition amount is Y2O3With Gd2O30.5 wt.% of the total mass of the mixed powder, ZrO2The addition amount is Y2O3With Gd2O30.1 wt.% of the total mass of the mixed powder;
(2) adding a dispersant castor oil and a solvent into the mixed powder obtained in the step (1) to perform roller ball milling, wherein the grinding ball is made of zirconia, the diameter of the grinding ball is 60mm, the ball milling speed is 300r/min, the ball milling time is 15h, and the solid content of the slurry is adjusted to be 55 wt.%; the adding amount of the dispersing agent is 1.5 wt% of the total mass of the mixed raw material powder, and the solvent is a mixed solution of butanone and absolute ethyl alcohol (the mass ratio of the butanone to the absolute ethyl alcohol is 0.8);
(3) sequentially adding a plasticizer, namely propylene carbonate and a binder, namely polyacrylic acid, into the slurry obtained in the step (2), wherein the addition amount of the plasticizer is 10 wt% of the total mass of the mixed raw material powder, and the addition amount of the binder is 10 wt% of the total mass of the mixed raw material powder, and continuing ball milling for 36 hours;
(4) filtering the slurry obtained in the step (3), and directly carrying out tape casting molding, wherein the first-stage drying temperature of the tape casting machine is 35 ℃, the second-stage drying temperature is 40 ℃, and the tape casting speed is 50cm/min, so as to obtain a ceramic biscuit;
(5) cutting the biscuit obtained in the step (4) into a wafer with the diameter of 78mm, stacking the wafer with the number of 60 layers, carrying out warm isostatic pressing on the obtained biscuit, cutting and shaping the edge of the biscuit in a laser cutting mode, and then degreasing;
(6) vacuum sintering the degreased blank in the step (5), keeping the sintering temperature at 1500 ℃, keeping the temperature for 5h, taking out the ceramic, naturally cooling to room temperature, adding the ceramic into 263K liquid nitrogen, and preserving in the liquid nitrogen for 3 h;
(7) taking out the ceramic from the liquid nitrogen, directly putting the ceramic into a vacuum sintering furnace, heating to 1500 ℃ at 30 ℃/min, heating to 1930 ℃ at 5 ℃/min, preserving heat for 10h, taking out the ceramic, naturally cooling to room temperature, annealing at 1500 ℃ for 10h, and naturally cooling to room temperature to obtain the 5G communication signal-based unshielded microcrystalline ceramic backboard.
The 5G signal test confirms that the microcrystalline ceramic backboard prepared in the embodiment has no shielding to 5G communication signals.
Claims (7)
1. A preparation method of a 5G communication signal based unshielded microcrystalline ceramic backboard is characterized by comprising the following specific steps:
(1) separately weigh high purity Y2O3Powder, high purity Gd2O3Powder and high-purity ZrO2Adding the powder into a ball milling tank, wherein Y is2O3The addition amount is Y2O3With Gd2O30.1-0.9 wt.% of the mixed powder, ZrO 22The addition amount is Y2O3With Gd2O30.1-2 wt.% of the mass of the mixed powder;
(2) adding a dispersing agent and a solvent into the mixed powder obtained in the step (1) for ball milling, wherein the ball milling rotation speed is 80-300 r/min, the ball milling time is 15-36 h, and the solid content of the slurry is adjusted to be 45-55 wt%; the adding amount of the dispersing agent is 0.4-1.5 wt% of the total mass of the mixed raw material powder;
(3) sequentially adding a plasticizer and a binder into the slurry obtained in the step (2), wherein the addition amount of the plasticizer is 5-10 wt% of the total mass of the mixed raw material powder, and the addition amount of the binder is 5-10 wt% of the total mass of the mixed raw material powder, and continuing ball milling for 16-36 hours;
(4) filtering the slurry obtained in the step (3), and then directly carrying out tape casting to obtain a ceramic biscuit;
(5) carrying out custom cutting and stacking on the biscuit obtained in the step (4), carrying out warm isostatic pressing on the obtained biscuit, shaping the edge of the biscuit, and then degreasing;
(6) vacuum sintering the degreased blank in the step (5), wherein the sintering temperature is 1200-1500 ℃, the temperature is kept for 1-5 h, the ceramic is taken out, naturally cooled to room temperature, added into liquid nitrogen, and stored in the liquid nitrogen for 1-3 h;
(7) taking out the ceramic from the liquid nitrogen, directly putting the ceramic into a vacuum sintering furnace, heating to 1200-1500 ℃ at a speed of 10-30 ℃/min, heating to 1750-1930 ℃ at a speed of 1-5 ℃/min, preserving heat for 2-10 h, taking out the ceramic, naturally cooling to room temperature, annealing at an annealing temperature of 1100-1500 ℃ for 10-20 h, and naturally cooling to room temperature to obtain the 5G communication signal-based unshielded microcrystalline ceramic backboard.
2. The preparation method of the 5G communication signal-based unshielded microcrystalline ceramic backboard according to claim 1, wherein the ball milling in the step (2) is roller ball milling, the grinding balls are made of zirconia, and the diameter of the grinding balls is 20-80 mm.
3. The method for preparing a 5G communication signal-based unshielded microcrystalline ceramic back plate according to claim 1, wherein the dispersant in the step (2) is one or more of NP-10, herring oil and castor oil; the solvent is a mixed solution of butanone and absolute ethyl alcohol, and the mass ratio of the butanone to the absolute ethyl alcohol is 0.5-0.8.
4. The method for preparing a 5G communication signal based unshielded microcrystalline ceramic back plate according to claim 1, wherein the plasticizer in the step (3) is one or more of butyl benzyl phthalate, dibutyl phthalate and propylene carbonate.
5. The method for preparing a 5G communication signal-based unshielded microcrystalline ceramic back plate as claimed in claim 1, wherein the binder in the step (3) is one or more of polyvinyl butyral, ethyl methacrylate and polyacrylic acid.
6. The preparation method of the 5G communication signal based unshielded microcrystalline ceramic backboard according to claim 1, wherein the specific parameters of the tape casting process in the step (4) are as follows: the first-stage drying temperature of the casting machine is 25-35 ℃, the second-stage drying temperature is 30-40 ℃, and the casting speed is 10-50 cm/min.
7. The preparation method of the 5G communication signal based unshielded microcrystalline ceramic backboard according to claim 1, wherein the temperature of the liquid nitrogen in the step (6) is 213-263K.
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