阅读说明：本技术 高致密细晶粒陶瓷及其制备方法和应用 (High-density fine-grain ceramic and preparation method and application thereof ) 是由 任佳乐 旷峰华 张洪波 任瑞康 崔鸽 于 2020-12-31 设计创作，主要内容包括：本发明是关于一种高致密细晶粒陶瓷及其制备方法和应用。所述高致密细晶粒陶瓷的制备方法按照以下步骤烧结陶瓷素坯：将所述陶瓷素坯进行n次“升温,保温和降温”,其中,n为大于或者等于2的自然数；所述高致密细晶粒陶瓷的相对密度≥99％,晶粒尺寸≤10μm。所要解决的技术问题是如何制备一种高致密细晶粒的陶瓷,使所述陶瓷的相对密度≥99％,晶粒尺寸≤10μm；同时,所述方法使用现有技术中的设备即可完成陶瓷烧结,无需引入特殊设备,生产成本低,易于大批量生产和工业化推广,从而更加适于实用。(The invention relates to a high-density fine-grain ceramic and a preparation method and application thereof. The preparation method of the high-density fine-grain ceramic comprises the following steps of sintering ceramic biscuit: heating, preserving heat and cooling the ceramic biscuit for n times, wherein n is a natural number greater than or equal to 2; the relative density of the high-density fine-grain ceramic is more than or equal to 99 percent, and the grain size is less than or equal to 10 mu m. The technical problem to be solved is how to prepare the high-density fine-grain ceramic, so that the relative density of the ceramic is more than or equal to 99 percent, and the grain size is less than or equal to 10 mu m; meanwhile, the method can finish ceramic sintering by using equipment in the prior art, does not need to introduce special equipment, has low production cost, and is easy for mass production and industrial popularization, thereby being more suitable for practicality.)

1. The preparation method of the high-density fine-grain ceramic is characterized by sintering a ceramic biscuit according to the following steps: and (2) heating, preserving heat and cooling the ceramic biscuit n times, wherein n is a natural number greater than or equal to 2.

2. The method of claim 1, wherein the ceramic greenbody is sintered according to the following steps:

if n is 2, the steps are as follows:

1) first heating to T_max-1Keeping the temperature, and cooling to T DEG C_min-1℃；

2) The second heating up to T_max-2Keeping the temperature, and cooling to room temperature to obtain ceramic;

wherein, T_max-2>T_max-1；

If n is 3-5, the steps are as follows:

1') first temperature increase to T_max-1Keeping the temperature, and cooling to T DEG C_min-1℃；

2’)......；

3') heating to T for the n-1 th time_max-(n-1)Keeping the temperature, and cooling to T DEG C_min-(n-1)℃；

4') increasing the temperature to T for the nth time_max-nKeeping the temperature, and cooling to room temperature to obtain ceramic;

wherein, T is_max-1，T_max-2......，T_max-nOn a first line with a slope>0；

The T is_min-1，T_minx-2......，T_min-(n-1)And the slope of the second straight line is 0.

3. The production method according to claim 1 or 2, wherein the rate of temperature rise is 5 ℃/min to 100 ℃/min; the cooling speed is 5-100 ℃/min.

4. The method according to claim 1 or 2, wherein the process time of the heat preservation is 10min to 60 min.

5. The method of claim 2, wherein Δ T ═ T_max-n-T_max1And delta T is 10-50 ℃.

6. The method of claim 2, wherein T is_min-1，T_minx-2......，T_min-(n-1)Determined according to the material of the ceramic biscuit, which is equal to the creep temperature of the densified ceramic of said material.

7. A highly dense fine-grained ceramic produced by the method according to any one of claims 1 to 6, having a relative density of 99% or more and a grain size of 10 μm or less.

8. The high density fine grain ceramic of claim 7 wherein the ceramic biscuit is of alumina, zirconia toughened alumina, spinel, mullite, aluminum nitride or silicon nitride.

9. A thin film hybrid integrated circuit sealing module comprising a ceramic carrier substrate, wherein the ceramic carrier substrate is made of the high density fine grain ceramic of claim 8.

10. An IGBT module comprising a ceramic carrier substrate, wherein the ceramic carrier substrate is made of the high dense fine grain ceramic of claim 8.

11. A deep sea probe comprising a ceramic pipe and a ceramic sensor, wherein the ceramic pipe and the ceramic sensor are made of the high dense fine grain ceramic of claim 8.

12. An oil exploration device comprising a ceramic pipe and a ceramic impact head, wherein said ceramic pipe and said ceramic impact head are made using the high density fine grain ceramic of claim 8.

13. An engine comprising a ceramic bearing and a ceramic housing, wherein said ceramic bearing and said ceramic housing are made using the high density, fine grained ceramic of claim 8.

14. An artificial joint made by using the high-density fine-grained ceramic according to claim 8.

15. An artificial denture, wherein the artificial denture is made of the highly dense fine-grained ceramic according to claim 8.

Technical Field

The invention belongs to the technical field of high-performance ceramic manufacturing for the electronic industry, and particularly relates to high-density fine-grain ceramic and a preparation method and application thereof.

Background

The high-performance ceramic has a series of excellent characteristics of high strength, high hardness, high temperature resistance, corrosion resistance, wear resistance, stable chemical properties and the like, and is widely applied to the fields of aerospace, machinery, electronics, chemical industry, communication, energy, biomedicine, environmental engineering and the like.

In the prior art, high-performance ceramic sintering is generally carried out at high temperature in an atmospheric atmosphere, but the sintering process has the following problems. If the sintering rate is too high in the sintering process, the ceramic product has more residual pores and abnormally grown crystal grains, so that the compactness is lower and the mechanical property is poor; if the temperature rise rate is too slow, the sintering efficiency is too low, and the production cost is too high.

It is reported in literature that high-performance ceramics with high density, fine grains and high strength can be obtained by adopting an oscillating pressure sintering method and a two-step sintering method. The oscillating pressure sintering method is mainly characterized in that oscillating pressure is introduced in the sintering process, and then a high-density and high-strength ceramic blank is obtained. The two-step sintering method is that in the sintering process, the temperature is quickly increased to a very high temperature to obtain an initial density, then the temperature is quickly reduced to a certain higher temperature, and finally the ceramic blank with high density and fine grains is obtained after long-time heat preservation. However, the oscillating pressure sintering method and the two-step sintering method can be realized only by adopting special sintering equipment, so that the production cost is high, and the mass production and the industrial popularization and application are difficult.

Disclosure of Invention

The invention mainly aims to provide a high-density fine-grain ceramic and a preparation method and application thereof, and aims to solve the technical problem of how to prepare the high-density fine-grain ceramic, so that the relative density of the ceramic is more than or equal to 99 percent, and the grain size is less than or equal to 10 mu m; meanwhile, the method can finish ceramic sintering by using equipment in the prior art, does not need to introduce special equipment, has low production cost, and is easy for mass production and industrial popularization, thereby being more suitable for practicality.

The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. According to the preparation method of the high-density fine-grain ceramic provided by the invention, a ceramic biscuit is sintered according to the following steps: and (2) heating, preserving heat and cooling the ceramic biscuit n times, wherein n is a natural number greater than or equal to 2.

The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.

Preferably, the method of preparation, wherein the ceramic biscuit is sintered according to the following steps:

if n is 2, the steps are as follows:

1) first heating to T_max-1Keeping the temperature, and cooling to T DEG C_min-1℃；

2) The second heating up to T_max-2Keeping the temperature, and cooling to room temperature to obtain ceramic;

wherein, T_max-2>T_max-1；

If n is 3-5, the steps are as follows:

1') first temperature increase to T_max-1Keeping the temperature, and cooling to T DEG C_min-1℃；

2’)......；

3') heating to T for the n-1 th time_max-(n-1)Keeping the temperature, and cooling to T DEG C_min-(n-1)℃；

4') increasing the temperature to T for the nth time_max-nKeeping the temperature, and cooling to room temperature to obtain ceramic;

wherein, T is_max-1，T_max-2......，T_max-nOn a first line with a slope>0；

The T is_min-1，T_minx-2......，T_min-(n-1)And the slope of the second straight line is 0.

Preferably, in the preparation method, the temperature rise speed is 5 ℃/min to 100 ℃/min; the cooling speed is 5-100 ℃/min.

Preferably, in the preparation method, the process time of the heat preservation is 10min to 60 min.

Preferably, the aforementioned preparation method, wherein Δ T ═ T_max-n-T_max1And delta T is 10-50 ℃.

Preferably, the preparation method is as described above, wherein T is_min-1，T_minx-2......，T_min-(n-1)Determined according to the material of the ceramic biscuit, which is equal to the creep temperature of the densified ceramic of said material.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the high-density fine-grain ceramic prepared by the method, the relative density is more than or equal to 99%, and the grain size is less than or equal to 10 mu m.

The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.

Preferably, the ceramic biscuit is made of alumina, zirconia toughened alumina, spinel, mullite, aluminum nitride or silicon nitride.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The thin film hybrid integrated circuit sealing module provided by the invention comprises a ceramic bearing substrate, wherein the ceramic bearing substrate is made of the high-density fine-grain ceramic.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The IGBT module provided by the invention comprises a ceramic bearing substrate, wherein the ceramic bearing substrate is made of the high-density fine-grain ceramic.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The deep sea detection device provided by the invention comprises a ceramic pipeline and a ceramic sensor, wherein the ceramic pipeline and the ceramic sensor are made of the high-density fine-grain ceramic.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The oil exploration device provided by the invention comprises a ceramic pipeline and a ceramic impact head, wherein the ceramic pipeline and the ceramic impact head are made of the high-density fine-grain ceramic.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The engine provided by the invention comprises the ceramic bearing and the ceramic shell, wherein the ceramic bearing and the ceramic shell are made of the high-density fine-grain ceramic.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the artificial joint provided by the invention, the artificial joint is made of the high-density fine-grain ceramic.

The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the artificial denture provided by the invention, the artificial denture is made of the high-density fine-grain ceramic.

By the technical scheme, the high-density fine-grain ceramic and the preparation method and application thereof provided by the invention at least have the following advantages:

1. the invention provides high-density fine-grain ceramic and a preparation method and application thereof, ceramic biscuit is sintered by adopting an oscillation temperature sintering system, and the product has high performance: one is that the grain size of the ceramic body prepared by the method is small, especially the high-density fine grain ceramic prepared by 4 times of 'heating, heat preservation and cooling' process, the grain size of the alumina ceramic is reduced from 8 microns to 2 microns by 75 percent; the crystal grain of the zirconia toughened alumina ceramic is reduced from 5 microns to 0.8 microns by 84 percent; the crystal grains of the zirconia ceramic are reduced from 2 microns to 0.5 micron by 75 percent; the grain size of the aluminum nitride ceramic is reduced from 15 microns to 4 microns, and is reduced by 73.33%; the crystal grains of the silicon nitride ceramic are reduced from 12 microns to 3 microns, and are reduced by 75%; secondly, the density of the ceramic body prepared by the method is high, in particular to the high-density fine-grain ceramic prepared by adopting the 4-time 'heating, heat-preserving and cooling' process, and the density of the alumina ceramic is 3.9g/cm³Increased to 3.96g/cm³(ii) a The density of the zirconia toughened alumina ceramic is 4.2g/cm³Increased to 4.35g/cm³(ii) a The density of the zirconia ceramic is 5.95g/cm³Increased to 6.1g/cm³(ii) a The density of the aluminum nitride ceramic is 3.15g/cm³Increased to 3.3g/cm³(ii) a The density of the silicon nitride ceramic is 3.25g/cm³Increased to 3.4g/cm³(ii) a The relative density of the ceramics made of various materials is more than or equal to 99 percent; thirdly, the ceramic body prepared by the method has large bending strength, and particularly, the high-density fine-grain ceramic, alumina, prepared by 4 times of heating, heat preservation and cooling processesThe bending strength of the ceramic is increased from 425MPa to 607MPa, and is increased by 42.82%; the bending strength of the zirconia toughened alumina ceramic is increased from 625MPa to 751MPa by 20.16 percent; the bending strength of the zirconia ceramic is increased from 968MPa to 1376MPa, and is increased by 42.15 percent; the bending strength of the aluminum nitride ceramic is increased from 380MPa to 490MPa by 28.95 percent; the bending strength of the silicon nitride ceramic is increased from 805MPa to 1020MPa by 26.71 percent;

2. the high-density fine-grain ceramic and the preparation method and the application thereof provided by the invention adopt an oscillation temperature sintering system to sinter ceramic biscuit, and have high production efficiency; the sintering period is basically consistent with the conventional sintering period or is slightly shortened; compared with two-step sintering, one sintering period can be shortened by more than 30 h; in addition, the method does not involve temperature rise and temperature reduction at a limit rate, so that the sintering capacity of a single device can be improved by more than 3 times; compared with a vibration pressure sintering method, the method does not need an additional pressure device, and is more suitable for batch production; the single equipment for sintering by oscillating pressure can only sinter 1 piece or 1 piece at a time, but the invention can even realize continuous sintering, and the maximum productivity of the single equipment can be improved to 200 pieces/day;

3. according to the high-density fine-grain ceramic and the preparation method and application thereof, the conventional sintering equipment is adopted to complete the whole sintering process, no additional pressure device, heating device or any other auxiliary device is needed, the equipment is simple, the cost is low, and the large-scale production and the industrial popularization are easy to realize.

The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.

Drawings

FIG. 1 is a schematic representation of the oscillating temperature sintering curve proposed by the present invention.

Detailed Description

To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be made on a high-density fine-grained ceramic, a preparation method thereof, and specific embodiments, structures, characteristics and effects thereof according to the present invention with reference to the accompanying drawings and preferred embodiments.

The invention provides a preparation method of high-density fine-grain ceramic, which comprises the following steps of: and (2) heating, preserving heat and cooling the ceramic biscuit n times, wherein n is a natural number greater than or equal to 2.

Preferably, the ceramic biscuit is sintered according to the following steps: if n is 2, the steps are as follows: 1) first heating to T_max-1Keeping the temperature, and cooling to T DEG C_min-1DEG C; 2) the second heating up to T_max-2Keeping the temperature, and cooling to room temperature to obtain ceramic; wherein, T_max-2>T_max-1。

Preferably, the ceramic biscuit is sintered according to the following steps: if n is 3-5, the steps are as follows: 1') first temperature increase to T_max-1Keeping the temperature, and cooling to T DEG C_min-1DEG C; 2...; 3') heating to T for the n-1 th time_max-(n-1)Keeping the temperature, and cooling to T DEG C_min-(n-1)DEG C; 4') increasing the temperature to T for the nth time_max-nKeeping the temperature, and cooling to room temperature to obtain ceramic; wherein, T is_max-1，T_max-2......，T_max-nOn a first line with a slope>0; the T is_min-1，T_minx-2......，T_min-(n-1)And the slope of the second straight line is 0.

As shown in FIG. 1, the curve 1 is the high point temperature (T) of each temperature rise_max-1，T_max-2......，T_max-n) I.e. the first straight line mentioned above; curve 2 represents the oscillating temperature sintering curve of the present invention; curve 3 represents the sintering curve in the conventional sintering process; curve 4 is the low point temperature (T) for each ramp_min-1，T_minx-2......，T_min-(n-1)) I.e. the second straight line mentioned above.

In the heating, heat preservation and cooling process during the sintering of the ceramic biscuit, the temperature water level reached by each heating is higher than the temperature level reached by the last heating, and the parameter setting aims at ensuring that crystal grains are subjected to each heatingThe growth can obtain larger interface driving force than the previous growth; furthermore, in order to simplify the setting of the sintering process, the temperature level reached by each time of temperature rise is limited to increase in a linear relation in the technical scheme of the invention, namely, T is required_max-1，T_max-2......，T_max-nAfter connection, the two lines are in the same straight line, and the slope of the straight line>0. The purpose of each cooling is to release energy from the grains, so as to form a compressive stress on the ceramic, wherein the existence of the compressive stress can inhibit the abnormal growth of the grains, so that the ceramic can be densified after sintering; the temperature level reached by each temperature reduction is at the same level, namely T is required_min-1，T_minx-2......，T_min-(n-1)After connection, the two straight lines are on the same straight line, and the slope of the straight line is equal to 0.

The times n of heating, heat preservation and cooling are not too many, and the reasons are that: on one hand, the maximum temperature of ceramic sintering is limited, and can not be increased without limit; the temperature level of the heat preservation step of heating, heat preservation and cooling is gradually increased; if the circulation times are too many, the temperature level difference of two adjacent heat-preservation steps is small, and the technical effect that crystal grains grow under the driving force of an interface due to the temperature rise required in the process setting of temperature rise, heat preservation and temperature reduction and are passivated and compacted under the compressive stress through the temperature reduction is difficult to realize; on the other hand, too many times n of 'heating up, heat preservation and cooling down' can also prolong the time of the sintering process, and the comprehensive cost performance is not good.

Preferably, the temperature rising speed is 5 ℃/min to 100 ℃/min; the cooling speed is 5-100 ℃/min.

The heating speed and the cooling speed are not suitable to be too slow, because when the heating or cooling speed is too slow, the heat preservation time is prolonged equivalently, the clear division of the circulation stages of heating, heat preservation and cooling every time is not facilitated, and the method is difficult to realize that the interface driving force is provided by heating to grow the crystal grains and the pressure stress is provided by cooling to passivate the crystal grain interface to densify the crystal grains; when the temperature rise or the temperature drop speed is too high, firstly, the processing equipment can not endure and needs to use special equipment, so that the cost is not economical, and secondly, the ceramic can generate thermal stress and is not beneficial to the performance. In the technical scheme of the invention, the preferable temperature rise speed and temperature drop speed are 5-100 ℃/min.

Preferably, the speed of each temperature rise is equal; the cooling speed is equal each time; the absolute value of the temperature rising speed is equal to the absolute value of the temperature reducing speed. The purpose of this arrangement is to simplify the sintering temperature profile of the ceramic.

Preferably, the process time of the heat preservation is 10 min-60 min.

Preferably, the process time is equal for each incubation. The purpose of this arrangement is to simplify the sintering temperature profile of the ceramic.

The heat preservation time in the process of heating, heat preservation and cooling is set to be 10-60 min each time, on one hand, the process has enough time to ensure that the process has better compactness; if the heat preservation time is less than 10min, the prepared ceramic may not be compact; on the other hand, the abnormal growth of crystal grains caused by over-burning is avoided; if the heat preservation time is longer than 60min, the prepared ceramic has the possibility of abnormal grain growth.

The heat preservation duration in each heating, heat preservation and cooling process can be set to be consistent with the heat preservation time, and the purpose is to reduce the complexity of the process.

Preferably, Δ T ═ T_max-n-T_max1And delta T is 10-50 ℃.

In the technical scheme of the invention, the ceramic sintered T_max1Set to the process temperature at which the ceramic is conventionally sintered, and T_max-nIs set higher than T_max1The temperature is 10-50 ℃. Will T_max1The process temperature is set as the process temperature of conventional sintering of the ceramic, and the purpose is to ensure that the ceramic can be smoothly sintered under the temperature condition and obtain enough interface driving force to enable the crystal grains to grow; and T_max-nAnd T_max1The temperature difference is set to be 10-50 ℃, and the purpose is to control the sintering temperature of the ceramic within a certain temperature range so as to avoidThe ceramic is over-sintered, so that crystal grains of the ceramic grow excessively, and the strength of the ceramic is reduced.

In the technical scheme of the invention, clear boundary lines need to be kept between the heating, heat preservation and cooling and the next adjacent heating, heat preservation and cooling so as to obtain a better oscillation temperature effect.

Preferably, the temperature difference between two adjacent heat preservation steps is more than or equal to 10 ℃.

Preferably, the temperature difference between two adjacent heat preservation steps is more than or equal to 15 ℃.

Preferably, the temperature difference between two adjacent heat preservation steps is 15-20 ℃.

Preferably, said T is_min-1，T_minx-2......，T_min-(n-1)Determined according to the material of the ceramic biscuit, which is equal to the creep temperature of the densified ceramic of said material.

The creep temperature is the characteristic of the ceramic, and the creep temperature of various ceramics can be checked without an engineering book in the technical field of the ceramics at present, and generally is an empirical value.

According to the technical scheme, the creep temperature of the ceramic product with the same density and the same material prepared by the traditional sintering process is actually measured according to the density of the densified ceramic to be obtained. When a sintering process is formulated, the creep temperature of the detected material and the detected compactness is set as T in a sintering curve of the technical scheme of the invention_min-1，T_minx-2......，T_min-(n-1)。

The method for detecting the creep temperature of the ceramic comprises the following steps: preparing ceramic into a sample strip with the specification of 3mm multiplied by 4mm multiplied by 35mm, applying 100N-300N rated load to the sample strip by adopting a three-point bending method while heating in a high-temperature mechanical property system, and measuring a sample strip under the rated load; when the sample strip is plastically deformed at a certain temperature, the temperature is the creep temperature point of the sample strip. The creep temperature point can be read directly from the emergency strain curve.

The invention also provides the high-density fine-grain ceramic prepared by the method, wherein the relative density is more than or equal to 99 percent, and the grain size is less than or equal to 10 mu m.

The detection method of the relative density comprises the following steps: firstly, measuring the actual density value of the high-density fine-grain ceramic; then, looking up the theoretical density value of the material ceramic according to a standard table; the ratio of the actual density value to the theoretical density value is used as the relative density of the high-density fine-grain ceramic, and the relative density is expressed in unit percent.

Preferably, the ceramic biscuit is made of alumina, zirconia toughened alumina, spinel, mullite, aluminum nitride or silicon nitride.

The technical scheme of the invention can be suitable for sintering various ceramics, and the ceramics prepared by the oscillating temperature sintering method of the invention.

When n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by more than or equal to 6 percent.

When n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by more than or equal to 12 percent.

When n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by more than or equal to 20 percent.

When the ceramic is made of alumina and n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 8.24%; when n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 31.76%; when n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 42.82%.

When the material of the ceramic is zirconia toughened alumina and n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 6.40 percent; when n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 12.32 percent; when n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 20.16 percent.

When the material of the ceramic is zirconia and n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 9.71 percent; when n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 22.11 percent; when n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 42.15 percent.

When the ceramic is made of aluminum nitride and n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 8.16 percent; when n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 19.21 percent; when n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 28.95 percent.

When the ceramic is made of silicon nitride and n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 8.32%; when n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 19.25 percent; when n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 26.71 percent.

When n is 2, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by more than or equal to 25 percent.

When n is 3, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by more than or equal to 50 percent.

When n is 4, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by more than or equal to 73 percent.

When the ceramic is made of alumina and n is 2, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 37.5%; when n is 3, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 62.5 percent; when n is 4, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 75 percent.

When the material of the ceramic is zirconia toughened alumina, and n is 2, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 40%; when n is 3, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 70%; when n is 4, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 84 percent.

When the material of the ceramic is zirconia and n is 2, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 25%; when n is 3, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 50%; when n is 4, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 75 percent.

When the ceramic is made of aluminum nitride, and n is 2, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 33.33%; when n is 3, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 53.33%; when n is 4, the grain size of the high-density fine-grain ceramic prepared by the method is reduced by 73.33%.

When the ceramic is made of silicon nitride and n is 2, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 25%; when n is 3, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 50 percent; when n is 4, the mechanical strength of the high-density fine-grain ceramic prepared by the method is improved by 75 percent.

When n is 2, the density of the high-density fine-grain ceramic product prepared by the method is improved by more than or equal to 1.03 percent.

When n is 3, the density of the high-density fine-grain ceramic product prepared by the method is improved by more than or equal to 1.28 percent.

When n is 4, the density of the high-density fine-grain ceramic product prepared by the method is improved by more than or equal to 1.54 percent.

When the ceramic is made of alumina and n is 2, the density of the high-density fine-grain ceramic product prepared by the method is improved by 1.03%; when n is 3, the density of the high-density fine-grain ceramic prepared by the method is improved by 1.28 percent; when n is 4, the product density of the high-density fine-grain ceramic prepared by the method is improved by 1.54 percent.

When the ceramic is made of zirconia toughened alumina and n is 2, the density of the high-density fine-grain ceramic product prepared by the method is increased by 2.62%; when n is 3, the density of the high-density fine-grain ceramic prepared by the method is improved by 3.57 percent; when n is 4, the product density of the high-density fine-grain ceramic prepared by the method is improved by 3.57 percent.

When the ceramic is made of zirconia and n is 2, the density of the high-density fine-grain ceramic product prepared by the method is improved by 1.68%; when n is 3, the density of the high-density fine-grain ceramic prepared by the method is improved by 2.52 percent; when n is 4, the product density of the high-density fine-grain ceramic prepared by the method is improved by 2.52 percent.

When the ceramic is made of aluminum nitride, and n is 2, the density of the high-density fine-grain ceramic product prepared by the method is improved by 3.81%; when n is 3, the product density of the high-density fine-grain ceramic prepared by the method is improved by 4.13 percent; when n is 4, the product density of the high-density fine-grain ceramic prepared by the method is improved by 4.76%.

When the ceramic is made of silicon nitride, and n is 2, the density of the high-density fine-grain ceramic product prepared by the method is improved by 3.69%; when n is 3, the product density of the high-density fine-grain ceramic prepared by the method is improved by 4.00 percent; when n is 4, the product density of the high-density fine-grain ceramic prepared by the method is improved by 4.62 percent.

When n is 5, the density of the ceramics made of various materials is more than or equal to 99 percent, the grain size is less than or equal to 10 mu m, the mechanical property is good, but the process time can be correspondingly prolonged and the improvement of the comprehensive performance is limited when the temperature rise, the heat preservation and the temperature reduction are increased once. Furthermore, in the technical scheme of the invention, n is preferably 3 times or 4 times. Furthermore, in the technical scheme of the invention, n is preferably 3 times or 4 times.

The invention also provides a thin film hybrid integrated circuit sealing module which comprises a ceramic bearing substrate, wherein the ceramic bearing substrate is made of the high-density fine-grain ceramic.

The invention further provides an IGBT module which comprises a ceramic bearing substrate, wherein the ceramic bearing substrate is made of the high-density fine-grain ceramic. The IGBT is an abbreviation of Insulated Gate Bipolar Transistor and refers to an Insulated Gate Bipolar Transistor.

The invention also provides a deep sea detection device which comprises a ceramic pipeline and a ceramic sensor, wherein the ceramic pipeline and the ceramic sensor are made of the high-density fine-grain ceramic.

The invention also provides an oil exploration device which comprises a ceramic pipeline and a ceramic impact head, wherein the ceramic pipeline and the ceramic impact head are made of the high-density fine-grain ceramic.

The invention also provides an engine which comprises the ceramic bearing and the ceramic shell, wherein the ceramic bearing and the ceramic shell are made of the high-density fine-grain ceramic.

The invention also provides an artificial joint which is made of the high-density fine-grain ceramic.

The invention also provides an artificial denture which is made of the high-density fine-grain ceramic.

The technical solution of the present invention is explained in detail by the following more specific examples. Unless otherwise stated, the detection of the properties is carried out by detection methods customary in the art.

Examples 1 to 1

The ceramic biscuit is made of alumina. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1500 ℃, the temperature is kept for 30min, the first temperature drop speed is 5 ℃/min, and the temperature is reduced to 1400 ℃.

And the second temperature rising speed is 5 ℃/min, the temperature rises to 1550 ℃, the temperature is kept for 60min, the second temperature lowering speed is 5 ℃/min, and the temperature is lowered to the room temperature, so that the high-density fine-grain ceramic is obtained.

The density of the high-density fine-grained ceramic in the embodiment is 3.94g/cm through detection³The relative density is 98.99%; the average grain size was 5 μm; the bending strength was 460 MPa.

Examples 1 to 2

The ceramic biscuit is made of alumina. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1500 ℃, the temperature is kept for 30min, the first temperature drop speed is 100 ℃/min, and the temperature is reduced to 1400 ℃.

The second temperature rise speed is 100 ℃/min, the temperature is raised to 1530 ℃, the temperature is kept for 30min, the second temperature drop speed is 100 ℃/min, and the temperature is reduced to 1400 ℃.

And the third temperature rise speed is 100 ℃/min, the temperature is raised to 1550 ℃, the temperature is kept for 10min, the third temperature drop speed is 5 ℃/min, and the temperature is reduced to the room temperature, so that the high-density fine-grain ceramic is obtained.

The density of the high-density fine-grain ceramic is 3.95g/cm through detection³The relative density is 99.25%; the average grain size was 3 μm; the flexural strength was 560 MPa.

Examples 1 to 3

The ceramic biscuit is made of alumina. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1500 ℃, the temperature is kept for 30min, the first temperature drop speed is 20 ℃/min, and the temperature is reduced to 1400 ℃.

The second temperature rise speed is 10 ℃/min, the temperature rises to 1515 ℃, the temperature is preserved for 10min, the second temperature reduction speed is 50 ℃/min, and the temperature is reduced to 1400 ℃.

The third temperature rise speed is 100 ℃/min, the temperature rises to 1535 ℃, the temperature is preserved for 10min, the third temperature drop speed is 100 ℃/min, and the temperature is reduced to 1400 ℃.

And the fourth temperature rising speed is 100 ℃/min, the temperature rises to 1550 ℃, the temperature is preserved for 10min, the fourth temperature lowering speed is 5 ℃/min, and the temperature is lowered to the room temperature, so that the high-density fine-grain ceramic is obtained.

The density of the high-density fine-grain ceramic is 3.96g/cm through detection³The relative density is 99.50%; the average grain size was 2 μm; the bending strength was 607 MPa.

Comparative example 1

The ceramic biscuit is made of alumina. The shaking sintering system is as follows:

heating to 1500 deg.C/min at a rate of 5 deg.C/min, maintaining for 120min at a rate of 5 deg.C/min, and cooling to room temperature to obtain the final product.

The density of the ceramic of this comparative example was found to be 3.90g/cm³The relative density is 97.99%; the average grain size was 8 μm;the flexural strength was 425 MPa.

Example 2-1

The ceramic biscuit is made of zirconia toughened alumina. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1550 ℃, the temperature is kept for 30min, the first temperature drop speed is 5 ℃/min, and the temperature is reduced to 1460 ℃.

And the second temperature rise speed is 5 ℃/min, the temperature is raised to 1600 ℃, the temperature is kept for 60min, the second temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grained ceramic in the embodiment is 4.31g/cm through detection³The relative density is 99.08%; the average grain size was 3 μm; the flexural strength was 665 MPa.

Examples 2 to 2

The ceramic biscuit is made of zirconia toughened alumina. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1550 ℃, the temperature is kept for 30min, the first temperature drop speed is 100 ℃/min, and the temperature is reduced to 1460 ℃.

The second temperature rise speed is 100 ℃/min, the temperature is raised to 1580 ℃, the temperature is kept for 30min, the second temperature reduction speed is 100 ℃/min, and the temperature is reduced to 1460 ℃.

And the third temperature rise speed is 100 ℃/min, the temperature is raised to 1600 ℃, the temperature is kept for 10min, the third temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grain ceramic is 4.35g/cm through detection³The relative density is 100%; the average grain size was 1.5 μm; the flexural strength was 702 MPa.

Examples 2 to 3

The ceramic biscuit is made of zirconia toughened alumina. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1550 ℃, the temperature is kept for 30min, the first temperature drop speed is 20 ℃/min, and the temperature is reduced to 1460 ℃.

The second temperature rise speed is 10 ℃/min, the temperature is raised to 1565 ℃, the temperature is kept for 10min, the second temperature drop speed is 50 ℃/min, and the temperature is reduced to 1460 ℃.

The third temperature rise speed is 100 ℃/min, the temperature is raised to 1585 ℃, the temperature is preserved for 10min, the third temperature reduction speed is 100 ℃/min, and the temperature is reduced to 1460 ℃.

And the fourth temperature rise speed is 100 ℃/min, the temperature is raised to 1600 ℃, the temperature is kept for 10min, the fourth temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grain ceramic is 4.35g/cm through detection³The relative density is 100%; the average grain size was 0.8 μm; the bending strength was 751 MPa.

Comparative example 2

The ceramic biscuit is made of zirconia toughened alumina. The shaking sintering system is as follows:

heating to 1550 deg.C/min at a rate of 5 deg.C/min, maintaining for 120min at a rate of 5 deg.C/min, and cooling to room temperature to obtain the final product.

The density of the ceramic of this comparative example was found to be 4.2g/cm³The relative density is 96.55%; the average grain size was 5 μm; the flexural strength was 625 MPa.

Example 3-1

The ceramic biscuit is made of zirconia. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1480 ℃, the temperature is preserved for 30min, the first temperature drop speed is 5 ℃/min, and the temperature is reduced to 1350 ℃.

The second temperature rise speed is 5 ℃/min, the temperature rises to 1530 ℃, the temperature is kept for 60min, the second temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grain ceramic is obtained.

The density of the high-density fine-grain ceramic in the embodiment is 6.05g/cm through detection³The relative density is 99.18%; the average grain size was 1.5 μm; the bending strength was 1062 MPa.

Examples 3 to 2

The ceramic biscuit is made of zirconia. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1480 ℃, the temperature is preserved for 30min, the first temperature reduction speed is 100 ℃/min, and the temperature is reduced to 1350 ℃.

The second temperature rise speed is 100 ℃/min, the temperature is raised to 1510 ℃, the temperature is preserved for 30min, the second temperature drop speed is 100 ℃/min, and the temperature is reduced to 1350 ℃.

And the third temperature rise speed is 100 ℃/min, the temperature is raised to 1530 ℃, the temperature is kept for 10min, the third temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grain ceramic in the embodiment is 6.1g/cm through detection³The relative density is 100%; the average grain size is 1 μm; the bending strength was 1182 MPa.

Examples 3 to 3

The ceramic biscuit is made of zirconia. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1480 ℃, the temperature is preserved for 30min, the first temperature drop speed is 20 ℃/min, and the temperature is reduced to 1350 ℃.

The second temperature rise speed is 10 ℃/min, the temperature is raised to 1495 ℃, the temperature is kept for 10min, the second temperature drop speed is 50 ℃/min, and the temperature is reduced to 1350 ℃.

The third temperature rise speed is 100 ℃/min, the temperature rises to 1515 ℃, the temperature is preserved for 10min, the third temperature drop speed is 100 ℃/min, and the temperature is reduced to 1350 ℃.

And the fourth temperature rise speed is 100 ℃/min, the temperature is raised to 1530 ℃, the temperature is kept for 10min, the fourth temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grain ceramic in the embodiment is 6.1g/cm through detection³The relative density is 100%; the average grain size was 0.5 μm; the flexural strength was 1376 MPa.

Comparative example 3

The ceramic biscuit is made of zirconia. The shaking sintering system is as follows:

heating to 1480 deg.C at a rate of 5 deg.C/min, maintaining for 120min at a rate of 5 deg.C/min, and cooling to room temperature to obtain the final product.

The density of the ceramic of this comparative example was found to be 5.95g/cm³The relative density is 97.54%; the average grain size was 2 μm; the bending strength was 968 MPa.

Example 4-1

The ceramic biscuit is made of aluminum nitride. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1750 ℃, the temperature is preserved for 30min, the first temperature drop speed is 5 ℃/min, and the temperature is reduced to 1300 ℃.

And the second temperature rise speed is 5 ℃/min, the temperature is raised to 1800 ℃, the temperature is kept for 60min, the second temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grain ceramic is obtained.

The density of the high-density fine-grained ceramic in the embodiment is 3.27g/cm through detection³The relative density is 99.09%; the average grain size was 10 μm; the flexural strength was 411 MPa.

Example 4 to 2

The ceramic biscuit is made of aluminum nitride. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1750 ℃, the temperature is preserved for 30min, the first temperature drop speed is 100 ℃/min, and the temperature is reduced to 1300 ℃.

The second temperature rise speed is 100 ℃/min, the temperature is raised to 1780 ℃, the temperature is kept for 30min, the second temperature drop speed is 100 ℃/min, and the temperature is reduced to 1300 ℃.

And the third temperature rise speed is 100 ℃/min, the temperature is raised to 1800 ℃, the temperature is kept for 10min, the third temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grained ceramic in the embodiment is 3.28g/cm through detection³The relative density is 99.39%; the average grain size was 7 μm; the flexural strength was 453 MPa.

Examples 4 to 3

The ceramic biscuit is made of aluminum nitride. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1750 ℃, the temperature is preserved for 30min, the first temperature drop speed is 50 ℃/min, and the temperature is reduced to 1300 ℃.

The second temperature rise speed is 10 ℃/min, the temperature rises to 1765 ℃, the temperature is kept for 10min, the second temperature drop speed is 50 ℃/min, and the temperature is reduced to 1300 ℃.

The third temperature rise speed is 100 ℃/min, the temperature is raised to 1785 ℃, the temperature is preserved for 10min, the third temperature reduction speed is 100 ℃/min, and the temperature is reduced to 1300 ℃.

And the fourth temperature rise speed is 100 ℃/min, the temperature is raised to 1800 ℃, the temperature is kept for 10min, the fourth temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grain ceramic is 3.3g/cm through detection³The relative density is 100%; the average grain size was 4 μm; the flexural strength was 490 MPa.

Comparative example 4

The ceramic biscuit is made of aluminum nitride. The shaking sintering system is as follows:

heating to 1750 deg.C at a rate of 5 deg.C/min, maintaining for 120min at a rate of 5 deg.C/min, and cooling to room temperature to obtain the final product.

The density of the ceramic of this comparative example was found to be 3.15g/cm³The relative density is 95.45%; the average grain size was 15 μm; the bending strength was 380 MPa.

Example 5-1

The ceramic biscuit is made of silicon nitride. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1850 ℃, the temperature is preserved for 30min, the first temperature drop speed is 50 ℃/min, and the temperature is reduced to 1350 ℃.

And the second temperature rise speed is 5 ℃/min, the temperature is raised to 1900 ℃, the temperature is kept for 60min, the second temperature drop speed is 5 ℃/min, and the temperature is reduced to room temperature, so that the high-density fine-grain ceramic is obtained.

The density of the high-density fine-grain ceramic in the embodiment is 3.37g/cm through detection³The relative density is 99.12%; the average grain size was 9 μm; the bending strength was 872 MPa.

Examples 5 and 2

The ceramic biscuit is made of silicon nitride. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1850 ℃, the temperature is preserved for 30min, the first temperature drop speed is 100 ℃/min, and the temperature is reduced to 1350 ℃.

The second temperature rise speed is 100 ℃/min, the temperature is raised to 1880 ℃, the temperature is kept for 30min, the second temperature drop speed is 100 ℃/min, and the temperature is reduced to 1350 ℃.

And the third temperature rise speed is 100 ℃/min, the temperature is raised to 1900 ℃, the temperature is kept for 10min, the third temperature drop speed is 5 ℃/min, and the temperature is reduced to the room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grained ceramic in the embodiment is 3.38g/cm through detection³The relative density is 99.41%; the average grain size was 6 μm; the bending strength was 960 MPa.

Examples 5 to 3

The ceramic biscuit is made of silicon nitride. The shaking sintering system is as follows:

the first temperature rise speed is 5 ℃/min, the temperature is raised to 1850 ℃, the temperature is preserved for 30min, the first temperature drop speed is 50 ℃/min, and the temperature is reduced to 1350 ℃.

The second temperature rise speed is 10 ℃/min, the temperature rises to 1865 ℃, the temperature is preserved for 10min, the second temperature drop speed is 50 ℃/min, and the temperature is reduced to 1350 ℃.

The third temperature rise speed is 100 ℃/min, the temperature is raised to 1885 ℃, the temperature is preserved for 10min, the third temperature drop speed is 100 ℃/min, and the temperature is reduced to 1350 ℃.

And the fourth temperature rise speed is 100 ℃/min, the temperature is raised to 1900 ℃, the temperature is kept for 10min, the fourth temperature drop speed is 5 ℃/min, and the temperature is reduced to the room temperature, so that the high-density fine-grained ceramic is obtained.

The density of the high-density fine-grain ceramic is 3.4g/cm through detection³The relative density is 100%; the average grain size was 3 μm; the bending strength was 1020 MPa.

Comparative example 5

The ceramic biscuit is made of silicon nitride. The shaking sintering system is as follows:

heating to 1850 deg.C at a rate of 5 deg.C/min, maintaining for 120min at a rate of 5 deg.C/min, and cooling to room temperature to obtain the final product.

The density of the ceramic of this comparative example was found to be 3.25g/cm³The relative density is 95.59%; the average grain size was 12 μm; the bending strength was 805 MPa.

The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.