Rapid high-temperature sintering method of compact block functional ceramic

Through the rapid high-temperature sintering method, the problems of element volatility and grain growth in ceramic materials at high temperatures in traditional sintering methods are solved, and densified sintering of ceramic materials is achieved, which improves mechanical properties and efficiency, while reducing energy consumption and cost. .

CN119462143APending Publication Date: 2025-02-18HUBEI UNIV
View PDF 1 Cites 0 Cited by

Patent Information

Application Number
CN202411695916.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-25
Publication Date
2025-02-18

AI Technical Summary

Technical Problem

Traditional sintering methods lead to excessive volatility of ceramic materials and abnormal growth of grains at high temperatures, affecting mechanical properties, and complex process, high cost, high energy consumption and low efficiency.

Method used

The rapid high-temperature sintering method is adopted, including raw material pretreatment, batching, pre-sintering, mixing, tableting and rapid sintering steps. The rapid sintering is achieved through a rapid heating furnace with an inert gas atmosphere, reducing sintering time and energy consumption.

Benefits of technology

It significantly reduces the sintering time, inhibits element volatility and grain growth, achieves densified sintering, improves the mechanical properties and efficiency of the ceramics, and reduces energy consumption and cost.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119462143A_ABST
    Figure CN119462143A_ABST
Patent Text Reader

Abstract

The invention discloses a rapid high-temperature sintering method for compact block functional ceramic, and the rapid high-temperature sintering method provided by the invention comprises the following steps: raw material pretreatment, burdening, pre-sintering, mixing, tabletting and rapid sintering. The lead zirconate titanate-based and potassium-sodium niobate-based piezoelectric ceramic has the advantages that the sintering time is obviously shortened, element volatilization and crystal grain growth are inhibited, the compact sintering of the lead zirconate titanate-based and potassium-sodium niobate-based piezoelectric ceramic is successfully realized, and the piezoelectric strain constants (d33) of PZT-1, PZT-2, KNN-1 and KNN-2 respectively reach 623, 334, 161 and 160pC / N. In addition, due to the small grain size and the compact structure, the dielectric loss is remarkably reduced, and meanwhile, the mechanical strength of the material is improved; the rapid high-temperature sintering method provided by the invention has the characteristics of low energy consumption, high efficiency and environmental protection.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of functional ceramic materials, and in particular to a method for rapid high-temperature sintering of dense block functional ceramics. Background Art

[0002] Functional ceramics usually include piezoelectric ceramics, optical ceramics, thermistor ceramics, ferroelectric ceramics, etc. Due to their unique electrical, magnetic, optical, thermal and other properties, they are widely used in modern industry and technology. Among them, piezoelectric ceramics are widely used in information communication, biomedicine, military and national defense, etc., and can be used to manufacture piezoelectric igniters, mobile X-ray power supplies, artillery detonation devices, underwater detection, non-destructive testing, ultrasonic cleaning, ultrasonic medical treatment, etc.; and with the development of new materials and performance improvement, its application range is still expanding. For example, potassium sodium niobate-based lead-free piezoelectric ceramics are non-toxic and environmentally friendly, and have gradually replaced traditional lead-containing piezoelectric ceramics in the fields of ultrasonic atomization and underwater acoustic transducer. Bismuth ferrite-barium titanate-based piezoelectric ceramics are the preferred materials for high-temperature piezoelectric vibration sensors due to their high Curie temperature, which can meet the application requirements in high-temperature extreme environments such as aerospace and nuclear energy.

[0003] Sintering is the core link in the preparation of piezoelectric ceramic materials, which involves the densification of ceramic powders, grain boundary formation and grain growth. In this process, we must not only ensure that the ceramic body is fully densified, but also accurately control its chemical composition to achieve controllable preparation of high-performance piezoelectric ceramics. Traditional sintering methods often cause excessive volatilization of ceramic powder elements due to their slow heating and cooling rates and long insulation time at high temperatures. In order to prevent the volatilization of elements during high-temperature sintering, buried powder sintering is usually required, which makes the process complex, costly, energy-intensive and inefficient. In addition, long-term high-temperature sintering will also cause abnormal growth of ceramic grains, thereby affecting the mechanical properties of the ceramics. For example, a Chinese patent (CN107573067A) discloses a low-temperature sintering method for a lead zirconate titanate-based piezoelectric ceramic sheet, comprising the following steps: mixing PbO raw material powder, ZrO2 raw material powder, TiO2 raw material powder and Sm2O3 raw material powder to obtain a mixed powder; ball milling, drying, and pre-sintering to obtain a pre-sintered powder; preparing a glass sintering aid LBBS by a quenching method, mixing the pre-sintered powder with the glass sintering aid, ball milling, drying, granulating, and pressing to obtain a piezoelectric ceramic green body; debinding and sintering the piezoelectric ceramic green body, the sintering temperature is 850°C, and the sintering time is 10 to 12 hours to obtain a piezoelectric ceramic sheet. Although the invention reduces the sintering temperature of the piezoelectric ceramic sheet from more than 1000°C to 850°C, which greatly reduces the volatilization of lead (melting point is 980°C), the sintering time is relatively long, which will cause abnormal growth of the ceramic grains, thereby affecting the mechanical properties of the ceramic. Therefore, there are still challenges in reducing energy consumption, reducing element volatilization and inhibiting abnormal grain growth, while achieving densification sintering of functional ceramics such as piezoelectric ceramics. Summary of the invention

[0004] In view of the deficiencies in the prior art, the object of the present invention is to provide a method for rapid high-temperature sintering of dense bulk functional ceramics, so as to achieve low-cost, low-energy consumption, and high-efficiency manufacturing of dense and high-performance bulk functional ceramics.

[0005] In order to achieve the above object, the present invention adopts the following technical scheme:

[0006] The present invention provides a method for rapid high-temperature sintering of dense block functional ceramics, comprising the following steps:

[0007] S1. Raw material pretreatment: before weighing, put Pb3O4 into an oven for drying or put K2CO3, Na2CO3, Li2CO3 into an oven for drying, and calcine ZrO2;

[0008] S2. Ingredients: weigh the raw materials Pb3O4, NiO, Nb2O5, ZrO2, TiO2, K2CO3, Na2CO3, Li2CO3, Nb2O5, Sb2O3, and Ta2O5 according to the stoichiometric ratio in the chemical formula of the bulk functional ceramic material, ball-mill the prepared raw materials, and mix them to obtain raw material powder;

[0009] S3, pre-calcining: pre-calcining the raw material powder at 880-950° C. for 2.5-3.5 hours to synthesize the acid salt compound, and cooling after the pre-calcining to obtain a pre-calcined powder;

[0010] S4, mixing: adding 0.01-1.5% of the mass of the pre-calcined powder to the pre-calcined powder and / or CuO, then ball milling and drying to obtain a mixed powder; wherein, when PbO and CuO are added at the same time, the sum of the mass of PbO and CuO accounts for 0.01-1.5% of the mass of the pre-calcined powder;

[0011] S5, tableting: adding polyvinyl alcohol glycerol aqueous solution to the mixed powder for granulation to obtain pellets, pressing the pellets into shapes and removing glue to obtain green sheets;

[0012] S6. Rapid sintering: placing the green sheet into a rapid heating furnace in an inert gas atmosphere for rapid sintering to obtain a bulk functional ceramic, wherein the rapid sintering heating rate is 50-200°C / s, the cooling rate is 10-100°C / s, the heat treatment temperature is 720-1050°C, the heat treatment time is 30s-20min, and the number of heat treatments is 1-20 times.

[0013] Preferably, in step S1, the temperature for drying the Pb3O4 is 115-125°C, and the time for drying the Pb3O4 is 11-13 hours.

[0014] Preferably, in step S1, the temperature for drying the K2CO3, Na2CO3 and Li2CO3 is 105-115°C, and the time for drying the K2CO3, Na2CO3 and Li2CO3 is 11-13h.

[0015] Preferably, in step S1, the temperature of calcining ZrO2 is 1150-1250°C, and the time of calcining ZrO2 is 1.5-2.5h.

[0016] Preferably, in step S2, the chemical formula is 0.355Pb(Ni 1 / 3 Nb2 / 3)O3-0.645Pb(Zr 0.41 Ti 0.59 )O3+1.5wt%(0.78PbO-0.22CuO) or [(K 0.43 Na0.57 ) 0.94 Li 0.06 ][(Nb 0.94 Sb 0.06 ) 0.95 Ta 0.05 ]O3-0.3mol%CuO.

[0017] Preferably, in step S2, the ball milling time is 1.5 to 3.5 hours.

[0018] Preferably, in step S4, the ball milling time is 3.5 to 4.5 hours.

[0019] Preferably, in step S5, the mass concentration of the polyvinyl alcohol glycerol aqueous solution is 4-6%, and the diameter of the green embryo sheet is 5-20 mm and the thickness is 0.5-2 mm.

[0020] Preferably, in step S5, the debinding temperature is 600-700°C.

[0021] Preferably, the inert gas is argon or nitrogen.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] (1) Compared with the traditional sintering method, the rapid high-temperature sintering method of dense block functional ceramics provided by the present invention significantly reduces the sintering time, inhibits the volatilization of elements and the growth of grains, and successfully realizes the densification sintering of lead zirconate titanate-based and potassium sodium niobate-based piezoelectric ceramics. Among them, the piezoelectric strain constant (d 33 ) are as high as 623, 334, 161, and 160 pC / N, respectively. In addition, its small grain size and dense structure not only significantly reduce the dielectric loss, but also help to improve its mechanical strength.

[0024] (2) The rapid high-temperature sintering method provided by the present invention has the characteristics of low energy consumption, high efficiency and environmental protection. Based on the Joule heating principle, the method of the present invention can accurately control the spatial distribution of temperature and the rapid heating rate, reduce energy dissipation, and reduce overall energy consumption; the extremely short sintering time inhibits the volatilization of harmful elements and improves the sintering efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 are scanning electron microscope photographs of PZT-1 in Example 1 of the present invention and PZT-1C in Comparative Example 1;

[0026] Figure 2 are scanning electron microscope photographs of PZT-2 in Example 2 of the present invention and PZT-2C in Comparative Example 2;

[0027] Figure 3 is the relative dielectric constant of PZT-1 in Example 1 of the present invention and PZT-1C in Comparative Example 1;

[0028] Figure 4 is the dielectric loss of PZT-1 in Example 1 of the present invention and PZT-1C in Comparative Example 1;

[0029] Figure 5 is the relative density of PZT-1 in Example 1 of the present invention and PZT-1C in Comparative Example 1. DETAILED DESCRIPTION

[0030] To make the purpose, technical scheme and advantages of the embodiment of the present invention clearer, the technical scheme in the embodiment of the present invention will be clearly and completely described below. If the specific conditions are not specified in the embodiment, it is carried out according to the normal conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified in the reagents or instruments used, they are all conventional products that can be purchased commercially. In addition, the technical schemes between the various embodiments can be combined with each other, but must be based on the ability of ordinary technicians in the field to achieve. When the combination of technical solutions is contradictory or cannot be achieved, it should be considered that the combination of such technical solutions does not exist, and is not within the scope of protection required by the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without making creative work belong to the scope of protection of the present invention.

[0031] The technical solution of the present invention is further described in detail below in conjunction with specific embodiments and drawings. It should be understood that the following embodiments are only used to explain the present invention, and are not used to limit the present invention.

[0032] Example 1

[0033] A method for rapid high-temperature sintering of dense bulk functional ceramics comprises the following steps:

[0034] (1) Raw material pretreatment: Before weighing, Pb3O4 was dried in an oven at 120°C for 12 h, and ZrO2 was calcined at 1200°C for 2 h;

[0035] (2) Ingredients: Pb3O4, NiO, Nb2O5, ZrO2, and TiO2 are used as raw materials, according to the chemical formula 0.355Pb(Ni 1 / 3 Nb 2 / 3 )O3-0.645Pb(Zr 0.41 Ti 0.59 )O3 to weigh the raw materials, ball-mill the prepared raw materials for 2 hours, and mix them thoroughly to obtain raw material powder;

[0036] (3) Pre-calcination: Pre-calcining the raw material powder at 880° C. for 3 h to synthesize the zirconate titanate compound, and cooling after the pre-calcination to obtain a pre-calcined powder;

[0037] (4) Mixing: Add 0.78 mol of PbO and 0.22 mol of CuO, which is 1.5% of the mass of the calcined powder, to the obtained calcined powder, and then ball mill for 4 h and dry to obtain a mixed powder;

[0038] (5) tabletting: adding a polyvinyl alcohol glycerol aqueous solution with a mass concentration of 5% to the obtained mixed powder for granulation; pressing the obtained granules into a mold and debinding at 650° C. to obtain a green embryo;

[0039] (6) Rapid sintering: The green body to be sintered was placed in a rapid heating furnace in an argon atmosphere for rapid sintering. The heating rate was 50°C / s, the cooling rate was 50°C / s, the heat treatment temperature was 953°C, the heat treatment time was 20 min, and the heat treatment number was 1. PZT-1 was obtained. Further test results showed that its piezoelectric strain constant d 33 It is 623pC / N.

[0040] Example 2

[0041] A method for rapid high-temperature sintering of dense bulk functional ceramics comprises the following steps:

[0042] (1) Raw material pretreatment: Before weighing, Pb3O4 was dried in an oven at 120°C for 12 h, and ZrO2 was calcined at 1200°C for 2 h;

[0043] (2) Ingredients: Pb3O4, NiO, Nb2O5, ZrO2, and TiO2 are used as raw materials, according to the chemical formula Pb(Zr 0.52 Ti 0.48 )O3 is weighed and mixed, and the prepared raw materials are ball-milled for 2 hours, and the raw material powder is obtained after being fully mixed;

[0044] (3) Pre-calcination: Pre-calcining the raw material powder at 880° C. for 3 h to synthesize the zirconate titanate compound, and cooling after the pre-calcination to obtain a pre-calcined powder;

[0045] (4) Mixing: Add 0.78 mol of PbO and 0.22 mol of CuO, which is 0.01% of the mass of the calcined powder, to the obtained calcined powder, and then ball mill for 4 h and dry to obtain a mixed powder;

[0046] (5) tabletting: adding a polyvinyl alcohol glycerol aqueous solution with a mass concentration of 5% to the obtained mixed powder for granulation; pressing the obtained granules into a mold and debinding at 650° C. to obtain a green embryo;

[0047] (6) Rapid sintering: The green body to be sintered was placed in a rapid heating furnace in an argon atmosphere for rapid sintering. The heating rate was 50°C / s, the cooling rate was 50°C / s, the heat treatment temperature was 947°C, the heat treatment time was 5 min, and the heat treatment number was 20 times. PZT-2 was obtained. Further test results showed that its piezoelectric strain constant d 33 It is 334pC / N.

[0048] Example 3

[0049] A method for rapid high-temperature sintering of dense bulk functional ceramics comprises the following steps:

[0050] (1) Raw material pretreatment: Before weighing, K2CO3, Na2CO3, and Li2CO3 were placed in an oven and dried at 110°C for 12 h;

[0051] (2) Ingredients: K2CO3, Na2CO3, Li2CO3, Nb2O5, Sb2O3, Ta2O5 are used as raw materials according to the chemical formula [(K 0.43 Na 0.57 ) 0.94 Li 0.06 ][(Nb 0.94 Sb 0.06 ) 0.95 Ta 0.05 ]O3-0.3mol%CuO is weighed and mixed, and the prepared raw materials are ball-milled for 3 hours, and the slurry is obtained after being fully mixed;

[0052] (3) Pre-calcination: Pre-calcining the raw material powder at 880° C. for 3 h to synthesize the zirconate titanate compound, and cooling after the pre-calcination to obtain a pre-calcined powder;

[0053] (4) Mixing: Add 0.78 mol of PbO and 0.22 mol of CuO, which is 0.01% of the mass of the calcined powder, to the obtained calcined powder, and then ball mill for 4 h and dry to obtain a mixed powder;

[0054] (5) tabletting: adding a polyvinyl alcohol glycerol aqueous solution with a mass concentration of 5% to the obtained mixed powder for granulation; pressing the obtained granules into a mold and debinding at 650° C. to obtain a green embryo;

[0055] (6) Rapid sintering: The green embryo to be sintered is placed in a rapid heating furnace in an argon atmosphere for rapid sintering. The heating rate is 200°C / s, the cooling rate is 100°C / s, the heat treatment temperature is 1050°C, the heat treatment time is 20 min, and the heat treatment number is 10 times. KNN-1 is obtained. Further test results show that its piezoelectric strain constant d 33 It is 161pC / N.

[0056] Example 4

[0057] A method for rapid high-temperature sintering of dense bulk functional ceramics comprises the following steps:

[0058] (1) Raw material pretreatment: Before weighing, K2CO3, Na2CO3, and Li2CO3 were placed in an oven and dried at 110°C for 12 h;

[0059] (2) Ingredients: K2CO3, Na2CO3, Li2CO3, Nb2O5, Sb2O3, Ta2O5 are used as raw materials according to the chemical formula [(K 0.43 Na 0.57 ) 0.94 Li 0.06 ][(Nb 0.94 Sb 0.06 ) 0.95 Ta 0.05 ]O3-0.01mol%CuO is weighed and mixed, the prepared raw materials are ball-milled for 3h, and the slurry is obtained after being fully mixed;

[0060] (3) Pre-calcination: Pre-calcining the powder obtained by drying at 950° C. for 3 h to synthesize the niobate compound, and cooling after the pre-calcination to obtain the pre-calcined powder;

[0061] (4) Mixing: Add 0.78 mol of PbO and 0.22 mol of CuO, which is 0.01% of the mass of the calcined powder, to the obtained calcined powder, and then ball mill and dry for 4 hours to obtain a mixed powder;

[0062] (5) tabletting: adding a polyvinyl alcohol glycerol aqueous solution with a mass concentration of 5% to the obtained mixed powder for granulation; pressing the obtained granules into a mold and debinding at 650° C. to obtain a green embryo;

[0063] (6) Rapid sintering: The green embryo to be sintered is placed in a rapid heating furnace in an argon atmosphere for rapid sintering, with a heating rate of 200°C / s, a cooling rate of 100°C / s, a heat treatment temperature of 720°C, a heat treatment time of 30s, and a heat treatment number of 1, to obtain KNN-2. Further test results show that its piezoelectric strain constant d 33 It is 160pC / N.

[0064] Comparative Example 1

[0065] A high temperature sintering method for piezoelectric ceramics comprises the following steps:

[0066] (1) Raw material pretreatment: Before weighing, Pb3O4 was dried in an oven at 120°C for 12 h, and ZrO2 was calcined at 1200°C for 2 h;

[0067] (2) Ingredients: Pb3O4, NiO, Nb2O5, ZrO2, and TiO2 are used as raw materials, according to the chemical formula 0.355Pb(Ni 1 / 3 Nb 2 / 3 )O3-0.645Pb(Zr 0.41 Ti 0.59 )O3 is weighed and mixed, and the prepared raw materials are ball-milled for 2 hours, and the raw material powder is obtained after being fully mixed;

[0068] (3) Pre-calcination: Pre-calcining the raw material powder at 880° C. for 3 h to synthesize the zirconate titanate compound, and cooling after the pre-calcination to obtain a pre-calcined powder;

[0069] (4) Mixing: Add 0.78 mol of PbO and 0.22 mol of CuO, which is 1.5% of the mass of the calcined powder, to the obtained calcined powder, and then ball mill for 4 h and dry to obtain a mixed powder;

[0070] (5) tabletting: adding a polyvinyl alcohol glycerol aqueous solution with a mass concentration of 5% to the obtained mixed powder for granulation; pressing the obtained granules into a mold and debinding at 650° C. to obtain a green embryo;

[0071] (6) Sintering: The debinded green body is placed in a box furnace for sintering at a sintering temperature of 1090°C and a sintering holding time of 4 h to finally obtain PZT-1C.

[0072] Comparative Example 2

[0073] A high temperature sintering method for piezoelectric ceramics comprises the following steps:

[0074] (1) Raw material pretreatment: Before weighing, Pb3O4 was dried in an oven at 120°C for 12 h, and ZrO2 was calcined at 1200°C for 2 h;

[0075] (2) Ingredients: Pb3O4, NiO, Nb2O5, ZrO2, and TiO2 are used as raw materials, according to the chemical formula 0.355Pb(Ni 1 / 3 Nb 2 / 3 )O3-0.645Pb(Zr 0.41 Ti 0.59 )O3 is weighed and mixed, and the prepared raw materials are ball-milled for 2 hours, and the raw material powder is obtained after being fully mixed;

[0076] (3) Pre-calcination: Pre-calcining the raw material powder at 880° C. for 3 h to synthesize the zirconate titanate compound, and cooling after the pre-calcination to obtain a pre-calcined powder;

[0077] (4) Mixing: Add 0.78 mol of PbO and 0.22 mol of CuO, which is 0.01% of the mass of the calcined powder, to the obtained calcined powder, and then ball mill for 4 h and dry to obtain a mixed powder;

[0078] (5) tabletting: adding a polyvinyl alcohol glycerol aqueous solution with a mass concentration of 5% to the obtained mixed powder for granulation; pressing the obtained granules into a mold and debinding at 650° C. to obtain a green embryo;

[0079] (6) Sintering: The debinded green body is placed in a box furnace for sintering at a sintering temperature of 1090°C and a sintering holding time of 4 h to finally obtain PZT-2C.

[0080] The specific formulas and abbreviations involved in each embodiment and comparative example are shown in Table 1 below.

[0081] Table 1 Sample formula and abbreviation

[0082]

[0083]

[0084] Test methods and results

[0085] The microstructure of the ceramic materials prepared in Example 1 and Comparative Example 1 was observed using an electron scanning microscope. Figure 1 ; The microscopic morphology of the ceramic materials prepared in Example 2 and Comparative Example 2 was observed using an electron scanning microscope, and the Figure 2 ; Test the relative dielectric constant values ​​of the ceramic materials in Example 1 and Comparative Example 1, and obtain Figure 3 ; The dielectric loss values ​​of the ceramic materials prepared in Example 1 and Comparative Example 1 were tested to obtain Figure 4 ; Test the relative density values ​​of the ceramic materials prepared in Example 1 and Comparative Example 1, and obtain Figure 5 .

[0086] Depend on Figure 1 and Figure 2 It can be seen that the dense bulk functional ceramic materials PZT-1 and PZT-2 prepared by rapid high temperature sintering in the present invention have the advantages of dense structure and small grain size; Figure 3 The dense bulk functional ceramic material PZT-1 prepared by rapid high temperature sintering in the present invention has a relative dielectric constant of up to 3177 when the sintering temperature is 953°C; Figure 4 It can be seen that the dense bulk functional ceramic material PZT-1 prepared by rapid high temperature sintering in the present invention has lower dielectric loss than the bulk functional ceramic material PZT-1C prepared by traditional sintering; Figure 5 It can be seen that the dense bulk functional ceramic material PZT-1 prepared by rapid high-temperature sintering in the present invention has a larger relative density and a higher density than the bulk functional ceramic material PZT-1C prepared by traditional sintering.

[0087] Finally, it should be noted that the above embodiments do not limit the present invention in any form. For those skilled in the art, some modifications and improvements can be made to the present invention. Therefore, any modification or improvement made without departing from the spirit of the present invention belongs to the scope of protection claimed in the present invention.

Claims

1. A method for rapid high temperature sintering of dense bulk functional ceramics, characterized in that: The following steps are involved: S1. Raw material pretreatment: before weighing, put Pb3O4 into an oven for drying or put K2CO3, Na2CO3, Li2CO3 into an oven for drying, and calcine ZrO2; S2. Ingredients: According to the chemical formula of the block functional ceramic material, weigh the raw materials Pb3O4, NiO, Nb2O5, ZrO2, TiO2, K2CO3, Na2CO3, Li2CO3, Nb2O5, Sb2O3, and Ta2O5, ball-mill the prepared raw materials, and mix them to obtain raw material powder; S3, pre-calcining: pre-calcining the raw material powder at 880-950° C. for 2.5-3.5 hours, and cooling after the pre-calcining to obtain a pre-calcined powder; S4, mixing: adding 0.01-1.5% of PbO and / or CuO by weight of the pre-calcined powder to the pre-calcined powder, then ball milling and drying to obtain a mixed powder; S5, tableting: adding polyvinyl alcohol glycerol aqueous solution to the mixed powder for granulation to obtain pellets, pressing the pellets into shapes and removing glue to obtain green sheets; S6. Rapid sintering: placing the green sheet into a rapid heating furnace in an inert gas atmosphere for rapid sintering to obtain a bulk functional ceramic, wherein the rapid sintering heating rate is 50-200°C / s, the cooling rate is 10-100°C / s, the heat treatment temperature is 720-1050°C, the heat treatment time is 30s-20min, and the number of heat treatments is 1-20 times.

2. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S1, the temperature of drying the Pb3O4 is 115-125°C, and the time of drying the Pb3O4 is 11-13 hours.

3. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S1, the temperature for drying the K2CO3, Na2CO3 and Li2CO3 is 105-115°C, and the time for drying the K2CO3, Na2CO3 and Li2CO3 is 11-13h.

4. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S1, the temperature of calcining ZrO2 is 1150-1250°C, and the time of calcining ZrO2 is 1.5-2.5h.

5. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S2, the chemical formula is 0.355Pb(Ni 1 / 3 Nb2 / 3)O3-0.645Pb(Zr 0.41 Ti 0.59 )O3+1.5wt%(0.78PbO-0.22CuO) or [(K 0.43 Na 0.57 ) 0.94 Li 0.06 ][(Nb 0.94 Sb 0.06 ) 0.95 Ta 0.05 ]O3-0.3mol%CuO.

6. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S2, the ball milling time is 1.5 to 3.5 hours.

7. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S4, the ball milling time is 3.5 to 4.5 hours.

8. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S5, the mass concentration of the polyvinyl alcohol glycerol aqueous solution is 4-6%, the diameter of the green embryo sheet is 5-20 mm, and the thickness is 0.5-2 mm.

9. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S5, the debinding temperature is 600-700°C.

10. The method for rapid high temperature sintering of dense block functional ceramics according to claim 1, characterized in that: In step S6, the inert gas is argon or nitrogen.

Citation Information

Patent Citations

  • Low-temperature sintering method of lead zirconate titanate-based piezoelectric ceramic piece

    CN107573067A