CN112248205B - Constant temperature and humidity drying method for composite material - Google Patents
Constant temperature and humidity drying method for composite material Download PDFInfo
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- CN112248205B CN112248205B CN202011119103.1A CN202011119103A CN112248205B CN 112248205 B CN112248205 B CN 112248205B CN 202011119103 A CN202011119103 A CN 202011119103A CN 112248205 B CN112248205 B CN 112248205B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/08—Humidity
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/10—Temperature; Pressure
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Ceramic Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Structural Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a constant temperature and humidity drying method of a composite material, which comprises the following steps: (1) when the weight of the composite material is increased by more than 60% after the gel reaction, firstly drying at constant temperature and humidity, keeping 70-90% of the saturation humidity at room temperature for 12-24h, keeping 50-70% of the saturation humidity for 12-24h, keeping 30-50% of the saturation humidity for 12-24h, finally drying normally, raising the temperature from room temperature to 250 ℃ within 2-5h, and keeping for 1-10 h; (2) when the weight of the composite material is increased by 20-60% after the gel reaction, keeping 50-70% of the saturation humidity for 12-24h, then keeping 30-50% of the saturation humidity for 12-24h, finally adopting common drying, raising the temperature from room temperature to 250 ℃ within 2-5h, and keeping for 1-10 h; (3) when the weight gain of the composite material is less than 20% after the gel reaction, the composite material is dried normally, the temperature is raised from room temperature to 250 ℃ within 2-5h, and the composite material is kept for 1-10 h. The drying method can ensure the continuity of the ceramic matrix, improve the performance of the composite material and compress and compound the preparation period of the composite material.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a constant-temperature constant-humidity drying process for a composite material.
Background
Constant temperature and humidity drying is an important process for preparing the composite material, and can reduce the stress of a ceramic matrix in the drying process and ensure the continuity and integrity of the matrix.
At present, the determination of a constant temperature and humidity system has no recyclable basis, only can be found out basically, and hardly has a guiding effect on the performance improvement of the composite material. In addition, the overlong constant temperature and humidity system can increase the preparation period and cost of the composite material.
Therefore, in view of the above disadvantages, it is desirable to provide an optimization method for a constant temperature and humidity drying process, which makes a basis for a constant temperature and humidity drying system, and can compress and compound the preparation cycle of the ceramic matrix under the condition of ensuring the continuity of the ceramic matrix and the performance of the composite material.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the technical problems that the determination of a constant temperature and humidity system has no recyclable basis, the performance of a composite material is difficult to guide, and the preparation period and the cost of the composite material are increased due to an overlong constant temperature and humidity system.
(II) technical scheme
In order to solve the technical problem, the invention provides a constant temperature and humidity drying method for a composite material in a first aspect, which comprises the following steps:
(1) when the weight of the composite material is increased by more than 60% after the gel reaction, adopting a first drying method;
(2) adopting a second drying method when the weight of the composite material is increased by 20-60% after the gel reaction;
(3) and when the weight of the composite material is increased by less than 20% after the gel reaction, adopting a third drying method.
Preferably, the first drying method is: drying at constant temperature and humidity, and then drying in a common way.
Preferably, the constant temperature and humidity drying step is as follows: firstly, at room temperature, keeping the humidity at 70-90% of the saturated humidity, and keeping the humidity for 12-24 h; then, changing the humidity to 50-70% of the saturated humidity, and keeping the humidity for 12-24 h; then, the humidity is changed to 30-50% of the saturated humidity, and the humidity is kept for 12-24 h.
Preferably, the step of ordinary drying is: the temperature is raised from room temperature to 250 ℃ within 2-5h and kept at the temperature for 1-10 h.
Preferably, the second drying method is: drying at constant temperature and humidity, and then drying in a common way.
Preferably, the constant temperature and humidity drying step is that the humidity is kept at 50-70% of the saturated humidity at room temperature and kept for 12-24 h; then, the humidity is changed to 30-50% of the saturated humidity, and the humidity is kept for 12-24 h.
Preferably, the step of ordinary drying is: the temperature is raised from room temperature to 250 ℃ within 2-5h and kept at the temperature for 1-10 h.
Preferably, the third drying method is: the temperature is raised from room temperature to 250 ℃ by using 2-5h and is kept at the temperature for 1-10 h.
Preferably, the composite material is one selected from the group consisting of an alumina fiber reinforced ceramic matrix composite, a quartz reinforced quartz composite, a carbon fiber reinforced carbon matrix composite, and a silicon carbide fiber reinforced silicon carbide composite.
The present invention provides, in a second aspect, a composite material obtainable by a process according to the first aspect of the invention; preferably, the performance of the composite material is improved by 15%.
(III) advantageous effects
The technical scheme of the invention has the following advantages:
(1) the continuity of the ceramic matrix can be guaranteed, and the performance of the composite material is improved by about 15%.
(2) The preparation period of the composite material can be shortened by over 30 percent under the condition of ensuring the continuity of the ceramic matrix and the performance of the composite material.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a constant temperature and humidity drying method of a composite material in a first aspect, which comprises the following steps:
(1) when the weight of the composite material is increased by more than 60% after the gel reaction, adopting a first drying method;
(2) adopting a second drying method when the weight of the composite material is increased by 20-60% after the gel reaction;
(3) and when the weight of the composite material is increased by less than 20% after the gel reaction, adopting a third drying method.
According to some preferred embodiments, the first drying method is: drying at constant temperature and humidity, and then drying in a common way.
According to some preferred embodiments, the drying step comprises: first, at room temperature (e.g., 20-30 ℃), the humidity is maintained at 70-90% (e.g., 70%, 80%, 90%) of the saturated humidity, and the humidity is maintained at this temperature for 12-24h (e.g., 12h, 15h, 18h, 20h, 22h, 24 h); then, the humidity is changed to 50-70% (e.g., 50%, 60%, 70%) of the saturated humidity, and the humidity is maintained for 12-24h (e.g., 12h, 15h, 18h, 20h, 22h, 24h) at the saturated humidity; then, the humidity is changed to 30-50% (e.g., 30%, 40%, 50%) of the saturation humidity, and the humidity is maintained for 12-24h (e.g., 12h, 15h, 18h, 20h, 22h, 24h) therein.
According to some preferred embodiments, the step of ordinary drying is: the temperature is raised from room temperature (e.g., 20-30 ℃) to 120-250 ℃ (e.g., 120 ℃, 150 ℃, 180 ℃, 200 ℃, 230 ℃, 250 ℃) within 2-5h, and is kept at the temperature for 1-10h (e.g., 1h, 3h, 5h, 8h, 10 h).
According to some preferred embodiments, the second drying method is: drying at constant temperature and humidity, and then drying in a common way.
According to some preferred embodiments, the constant temperature and humidity drying step is that the humidity is kept at 50-70% (e.g. 50%, 60%, 70%) of the saturation humidity at room temperature, and the humidity is kept at 12-24h (e.g. 12h, 15h, 18h, 20h, 22h, 24 h); then, the humidity is changed to 30-50% (e.g., 30%, 40%, 50%) of the saturation humidity, and the humidity is maintained for 12-24h (e.g., 12h, 15h, 18h, 20h, 22h, 24h) therein.
According to some preferred embodiments, the step of ordinary drying is: the temperature is raised from room temperature to 250 ℃ of 120-.
According to some preferred embodiments, the third drying method is: the temperature is raised from room temperature to 250 ℃ of 120 ℃ to 250 ℃ by using 2 to 5 hours (such as 120 ℃, 150 ℃, 180 ℃, 200 ℃, 230 ℃, 250 ℃) and is kept at the temperature for 1 to 10 hours (such as 1 hour, 3 hours, 5 hours, 8 hours and 10 hours).
According to some preferred embodiments, the composite material is selected from one of the group consisting of an alumina fiber reinforced ceramic matrix composite, a quartz reinforced quartz composite, a carbon fiber reinforced carbon based composite, and a silicon carbide fiber reinforced silicon carbide composite.
The present invention provides, in a second aspect, a composite material obtainable by a process according to the first aspect of the invention; preferably, the performance of the composite material is improved by 15%.
Example 1
The composite material of the fiber fabric is prepared by adopting a sol-gel method. A silica sol having a solid content of 35 mass% was prepared, and then a quartz fiber preform having a volume fraction of 45% was impregnated with the silica sol, and the impregnated quartz fiber preform was subjected to a gelling reaction at 50 ℃. After the gelling reaction, the wet composite material was weighed and the weight increased by 73% compared to the quartz fiber preform before impregnation. For the alumina fiber reinforced ceramic matrix composite material weighted after the gel reaction, constant temperature and humidity drying is firstly adopted, namely, at the temperature of 20 ℃, the humidity keeps 73% of the saturated humidity, and in the humidity range, the humidity keeps 12h, then the humidity is changed to 56% of the saturated humidity, and in the humidity, the humidity keeps 12h, then the humidity is changed to 32% of the saturated humidity, and in the humidity, the humidity keeps 12h, and finally, common drying is adopted, the temperature is increased from 20 ℃ to 120 ℃ within 2h, and the temperature keeps 1 h. The tensile strength of the composite was tested and is shown in table 1.
Example 2
The composite material of the fiber fabric is prepared by adopting a sol-gel method. A silica sol having a solid content of 35 mass% was prepared, and then an alumina fiber preform having a volume fraction of 45% was impregnated with the silica sol, and the impregnated alumina fiber preform was subjected to a gelling reaction at 50 ℃. After the gelling reaction, the wet composite material was weighed and the weight increased by 58% compared to the quartz fiber preform before impregnation. For the alumina fiber reinforced ceramic matrix composite material weighted after the gel reaction, constant temperature and humidity drying is firstly adopted, the humidity is kept to be 69% of the saturated humidity at the temperature of 25 ℃, the keeping time is 24h at the humidity, then the humidity is changed to be 47% of the saturated humidity, the humidity is kept for 24h at the humidity, and finally common drying is adopted, the temperature is increased from 25 ℃ to 250 ℃ within 5h, and the temperature is kept for 10 h. The tensile strength of the composite was tested and is shown in table 1.
Example 3
The composite material of the fiber fabric is prepared by adopting a sol-gel method. A silica sol having a solid content of 35 mass% was prepared, and then an alumina fiber preform having a volume fraction of 45% was impregnated with the silica sol, and the impregnated alumina fiber preform was subjected to a gelling reaction at 50 ℃. After the gelling reaction, weighing the wet composite material, increasing the weight by 15% compared with the quartz fiber preform before soaking, and for the alumina fiber reinforced ceramic matrix composite material increased in weight after the gelling reaction, adopting common drying, raising the temperature from 30 ℃ to 200 ℃ within 3h, and keeping the temperature for 5 h. The tensile strength of the composite was tested and is shown in table 1.
Example 4
This example 4 is substantially the same as example 1 except that: the composite material is quartz reinforced quartz composite material. The tensile strength of the composite was tested and is shown in table 1.
Example 5
This example 5 is substantially the same as example 1 except that: the composite material is carbon fiber reinforced carbon-based composite material. The tensile strength of the composite was tested and is shown in table 1.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that: and (3) drying the alumina fiber reinforced ceramic matrix composite material weighted after the gel reaction at constant temperature and humidity, namely, keeping the humidity at 30% of the saturation humidity at 25 ℃ for 72 h. The tensile strength of the composite was tested and is shown in table 1.
Comparative example 2
Comparative example 2 is substantially the same as example 2 except that: and (3) drying the alumina fiber reinforced ceramic matrix composite material weighted after the gel reaction at constant temperature and humidity, namely keeping the humidity at 50% of the saturated humidity at 25 ℃ for 72 h. The tensile strength of the composite was tested and is shown in table 1.
Comparative example 3
Comparative example 3 is substantially the same as example 3 except that: and drying the alumina fiber reinforced ceramic matrix composite material weighted after the gel reaction at constant temperature and humidity, and keeping the humidity at 60 percent of the saturated humidity for 72 hours at the temperature of 25 ℃. The tensile strength of the composite was tested and is shown in table 1.
Comparative example 4
This comparative example 4 is substantially the same as example 1 except that: the alumina fiber reinforced ceramic matrix composite material which is added with 70 percent of weight after gel reaction is dried at constant temperature and humidity, the humidity is kept at 50 percent of the saturated humidity at the temperature of 20 ℃, the humidity is kept for 12 hours at the temperature, then the humidity is changed to 30 percent of the saturated humidity, the humidity is kept for 12 hours, finally, the common drying is adopted, the temperature is increased from 20 ℃ to 120 ℃ within 2 hours, and the temperature is kept for 1 hour. The tensile strength of the composite was tested and is shown in table 1.
Table 1: tensile Strength of composites obtained by drying in examples and comparative examples
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A constant temperature and humidity drying method for composite materials is characterized by comprising the following steps:
(1) when the weight of the composite material is increased by more than 60% after the gel reaction, adopting a first drying method;
(2) adopting a second drying method when the weight of the composite material is increased by 20-60% after the gel reaction;
(3) when the weight gain of the composite material is less than 20% after the gel reaction, adopting a third drying method;
the first drying method comprises the following steps: firstly, drying at constant temperature and constant humidity, and then, drying in a common way;
the constant temperature and humidity drying method in the first drying method comprises the following steps: firstly, at room temperature, keeping the humidity at 70-90% of the saturated humidity, and keeping the humidity for 12-24 h; then, changing the humidity to 50-70% of the saturated humidity, and keeping the humidity for 12-24 h; then, changing the humidity to 30-50% of the saturated humidity, and keeping the humidity for 12-24 h;
the second drying method comprises the following steps: firstly, drying at constant temperature and constant humidity, and then, drying in a common way;
the constant temperature and humidity drying step in the second drying method comprises the steps of keeping the humidity at 50-70% of the saturated humidity at room temperature, and keeping the humidity for 12-24 h; then, the humidity is changed to 30-50% of the saturated humidity, and the humidity is kept for 12-24 h.
2. The method of claim 1, wherein:
the ordinary drying steps are as follows: the temperature is raised from room temperature to 250 ℃ within 2-5h and kept at the temperature for 1-10 h.
3. The method of claim 1, wherein:
the third drying method comprises the following steps: the temperature is raised from room temperature to 250 ℃ by using 2-5h and is kept at the temperature for 1-10 h.
4. The method of claim 1, wherein:
the composite material is selected from one of the group consisting of an alumina fiber reinforced ceramic matrix composite, a quartz reinforced quartz composite, a carbon fiber reinforced carbon matrix composite and a silicon carbide fiber reinforced silicon carbide composite.
5. A composite material characterized by:
the composite material is made according to the method of any one of claims 1-4; the tensile strength of the composite material is improved by 15%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8481900B2 (en) * | 2009-11-25 | 2013-07-09 | Corning Incorporated | Methods for drying ceramic materials |
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