CN109456077A - A kind of preparation method with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support - Google Patents

A kind of preparation method with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support Download PDF

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CN109456077A
CN109456077A CN201811450158.3A CN201811450158A CN109456077A CN 109456077 A CN109456077 A CN 109456077A CN 201811450158 A CN201811450158 A CN 201811450158A CN 109456077 A CN109456077 A CN 109456077A
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crystal whisker
borate crystal
compression strength
magnesium borate
preparation
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陈善华
韩世虎
罗青松
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Chengdu Univeristy of Technology
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Chengdu Univeristy of Technology
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
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Abstract

The invention discloses a kind of methods prepared with the magnesium borate crystal whisker ceramic film support for being suitable for porosity and compression strength, and this method is using basic magnesium carbonate and boric acid as primary raw material, magnesium fluoride (MgF2) it is sintering aid, polyvinyl alcohol (PVA) is binder, and deionized water is solvent, comprising the following steps: is 1. weighed;2. ball mill mixing;3. 80 DEG C of dryings;4. compression moulding;5. 110 DEG C of dryings;6. being sintered.Compared with existing invention, on the basis of reservation fabricated in situ prepares magnesium borate crystal whisker porous ceramics, it is the MPa of 11.35 MPa ~ 14.51 that the present invention, which has prepared compression strength range, the magnesium borate crystal whisker porous ceramics that porosity ranges are 51.77% ~ 60.95%, on the one hand it solves the problems, such as that magnesium borate crystal whisker porous ceramics compression strength and porosity change are too big, on the other hand solves the problems such as preparing magnesium borate crystal whisker porous ceramics complex process with freezing injection molding and sol-gal process.

Description

It is a kind of with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support Preparation method
Technical field
The present invention relates to a kind of preparation side with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support Method, in particular to a kind of preparation method using solid sintering technology fabricated in situ magnesium borate crystal whisker porous ceramics.It is obtained porous Ceramics have suitable porosity and compression strength, and skeleton is made of high-intensitive magnesium borate crystal whisker.
Background technique
Porous ceramics has the high and low thermal conductivity of porosity, the height that higher-strength, thermal conductivity is low, thermal stability is good and excellent The advantages that warm nature energy, has very extensive application prospect in fields such as chemical industry, food, environmental protection and light industrys.Currently, in porous pottery In the preparation process of porcelain, due to the presence of hole, so that the compression strength decline of ceramics.It is common, when porosity is higher than 40% And compression strength is greater than the porous ceramics of 15MPa, can be described as high-intensitive high porous ceramic.
It is a kind of prepare high porosity growth in situ magnesium borate crystal whisker porous ceramics method (patent No.: 201410796726.0) disclose a kind of preparation method of freeze-drying fabricated in situ magnesium borate crystal whisker porous ceramics, the method Using basic magnesium carbonate and boric acid as raw material, nitrate be catalyst, sodium carboxymethylcellulose pyce is binder, polyacrylamide is dispersion Agent, by the processes such as ball milling mixing, slurry preparation, casting, orientation freezing, vacuum freeze drying, sintering and washing, preparation Magnesium borate crystal whisker porous ceramics is gone out.The shortcomings that invention, is:
1. having prepared high porosity ceramic, but without the compression strength of research ceramics;
2. using the processes such as vacuum freeze drying, washing, preparation process is more complex.
A kind of porous ceramics standby using the magnesium slag, coal ash for manufacturing and preparation method thereof (patent No.: 201710046131.7) Disclose a kind of method that compression moulding method prepares porous ceramics.The method is using magnesium slag, flyash as raw material, using quartz sand as bone Material, is mixed in a certain ratio, is successfully prepared porous ceramics through crushing, molding and sintering.The shortcomings that invention, is:
1. porous ceramics made from is not using magnesium borate crystal whisker as skeleton structure;
Porous ceramics hole rate and intensity made from 2. are lower.
A kind of growth in situ prepares the method (patent No.: 201310621570.8) open of magnesium borate crystal whisker porous ceramics Using inorganic magnesium salt and boric acid as raw material, inorganic nitrate is catalyst, boric acid has been made by ball mill mixing, compacting and sintering Magnesium whisker porous ceramics.The shortcomings that invention, is:
1. compression strength is lower;
2. the sintered heat insulating time needed for is longer.
A kind of collosol and gel-freeze drying process prepare alumina porous ceramic method (patent No.: 200610119248.5) one kind is disclosed using aluminium isopropoxide as presoma, and high temperature is lauched solution and obtains alumina sol, regulates and controls colloidal sol Solid content, is added forming agent, vacuum degassing after cast molding, and frozen drying is finally prepared by high temperature sintering Alumina porous ceramic.The shortcomings that invention, is:
1. the skeleton structure of alumina porous ceramic made from is not alumina whisker;
2. needing the processes such as colloidal sol and freeze-drying and sintering temperature being higher, preparation process is complicated.
A kind of porous silicon carbide ceramic and preparation method thereof (patent No.: 201510821800.4) discloses a kind of compacting The method that the method for forming prepares carborundum porous ceramics.The method is with silicon carbide, aluminium hydroxide, gas-phase silica, water, dispersing agent and glues Agent mixing is tied, slurry is obtained;Then it by slurry drying and moulding, is finally sintered in air atmosphere and carborundum porous ceramics is made. Disadvantage of this law is that:
1. obtained carborundum porous ceramics porosity is lower, and about 10%~40%;
2. sintering temperature is higher and temperature-rise period is complicated.
Prepare high-intensitive high porosity growth in situ magnesium borate crystal whisker porous ceramics method (patent No.: 201810144625.3) one kind is disclosed using basic magnesium carbonate and boric acid as raw material, and sodium pyrophosphate is sintering aid, polyvinyl alcohol For binder, the technology of magnesium borate crystal whisker porous ceramics is made by ball mill mixing, compacting and sintering.The shortcomings that invention It is:
1. the compression strength variation range of obtained porous ceramics is too big;
2. the porosity change range of obtained porous ceramics is too big.
Summary of the invention
Having one of the objects of the present invention is to provide one kind is suitable for porosity and compression strength magnesium borate crystal whisker ceramic membrane Mixing is pressed into green compact first and makes it have some strength by the preparation method of supporter, this method, then passes through high temperature sintering Directly obtain the porous ceramics that skeleton is made of magnesium borate crystal whisker.With other fabricated in situ magnesium borate crystal whisker porous ceramics method phases Than on the one hand the present invention is solved on the basis of reservation fabricated in situ prepares magnesium borate crystal whisker porous ceramics, using solid sintering technology On the other hand magnesium borate crystal whisker porous ceramics compression strength of having determined and the too big problem of porosity change range are solved with freezing Injection molding and sol-gal process prepare the problems such as magnesium borate crystal whisker porous ceramics complex process.
Technical solution is: a kind of preparation side with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support Method, for this method using basic magnesium carbonate and boric acid as primary raw material, magnesium fluoride is sintering aid, and polyvinyl alcohol is binder, go from Sub- water is solvent, comprising the following steps:
1. weighing;
2. ball mill mixing;
3. 80 DEG C of dryings;
4. compression moulding;
5. 110 DEG C of dryings;
6. being sintered.
Preferably, the basic magnesium carbonate, boric acid are 1:1.1~1:1.5 mixing by Mg:B molar ratio, magnesium fluoride contains Amount is the 1%~5% of basic magnesium carbonate and boric acid gross mass, and polyvinyl alcohol addition is basic magnesium carbonate and boric acid gross mass 5%, deionized water content is the 55.56% of basic magnesium carbonate and boric acid gross mass.
Preferably, planetary ball mill revolving speed is not less than 300 r/min in the ball mill mixing process, Ball-milling Time is 6h~10h.
Preferably, using constant pressure and dry in 80 DEG C of drying processes, drying time is 12 h~15h.
Preferably, the press-moulding die is cylindrical mold, material is carbon steel.Mixing quality is 15g~20g, The intensity of pressure is 100MPa, and green compact forming diameter and thickness are 22mm.
Preferably, using constant pressure and dry in 110 DEG C of drying processes, drying time is 6 h~10h.
Preferably, 600 DEG C are risen to from room temperature with the rate of 1~5 DEG C/min first in the sintering process, heat preservation 1h~ Then 3h rises to 900 DEG C with the rate of 5 DEG C/min and keeps the temperature 2h, last furnace cooling.
The second object of the present invention is to provide a kind of with suitable porosity and compression strength magnesium borate crystal whisker ceramic membrane The preparation method of supporter, skeleton structure are made of magnesium borate crystal whisker.
Technical solution is: it is suitable for porosity that one kind, which has, and compression strength magnesium borate crystal whisker ceramic film support is by above-mentioned Method be prepared.The compression strength of the magnesium borate crystal whisker ceramic film support is 11.35MPa~14.51MPa, porosity It is 51.77%~60.95%, skeleton structure is by monocline Mg2B2O5Phase and a small amount of three oblique MgB4O7Phase composition.
Compared with prior art, the beneficial effects of the present invention are:
The present invention solves the problems, such as that magnesium borate crystal whisker porous ceramics compression strength and porosity change range are too big.
The present invention solves the problems such as existing method and process for preparing magnesium borate crystal whisker porous ceramics is complicated, this method technique Simply, easy to operate, energy saving.
The present invention solves in the existing method for preparing magnesium borate crystal whisker porous ceramics preform blank by intensity restricted problem. In the existing method, the intensity for freezing green compact in injection molding and gel injection-moulding is low, and intensity is little after sintering.
The skeleton with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support prepared by the present invention, by boron Sour magnesium whisker is mutually bonded in three-dimensional space, overlaps row.
It is prepared by the present invention that there is suitable porosity and compression strength magnesium borate crystal whisker ceramic film support, it can not only be used for making pottery Supporter in porcelain film can be also used for the porous ceramics that environment is protected in purification.
Detailed description of the invention
Fig. 1 is XRD of the magnesium borate crystal whisker porous ceramics under different magnesium fluoride sintering aid contents prepared by the present invention Figure;
Fig. 2 is the microscopic appearance figure of 1 product of the embodiment of the present invention;
Fig. 3 is the microscopic appearance figure of 2 product of the embodiment of the present invention;
Fig. 4 is the microscopic appearance figure of 3 product of the embodiment of the present invention;
Fig. 5 is the microscopic appearance figure of 4 product of the embodiment of the present invention;
Fig. 6 is that the present invention implements product compression strength and porosity figure;
Specific embodiment
The present invention will be further described with reference to the accompanying drawings.
It is suitable for porosity and compression strength magnesium borate crystal whisker ceramic film support preparation method that one kind, which has, and this method is with alkali Formula magnesium carbonate and boric acid are main raw material(s), and magnesium fluoride is sintering aid, with polyvinyl alcohol adhesive etc., by weighing, ball milling It is more that mixing, compression moulding, drying and sintering process direct in-situ have synthesized the magnesium borate crystal whisker that skeleton is made of magnesium borate crystal whisker Hole ceramics, the specific steps are as follows:
Step 1, it is by mixing and mass content that basic magnesium carbonate, boric acid are 1:1.1~1:1.5 by Mg:B molar ratio Basic magnesium carbonate and the magnesium fluoride of boric acid gross mass 1%~5%, mass content are basic magnesium carbonate and boric acid gross mass 5% Polyvinyl alcohol, mass content are put into agate after being mixed for the deionized water of basic magnesium carbonate and boric acid gross mass 55.56% In spheroidal graphite tank, using planetary ball mill ball milling, the revolving speed of ball mill is 300r/min, and Ball-milling Time is 6h~10h.
Step 2, the good blank of ball milling is placed in oven and dried.Oven temperature is 80 DEG C in this step, and drying time is 12h~15h.
Step 3, the blank after weighing the above-mentioned drying of 15g~20g is placed in compression moulding in cylindrical mold, and the intensity of pressure is 100MPa, green compact forming diameter and thickness are 22mm.
Step 4, the green compact of compacting are placed in baking oven and are dried.Oven temperature is 110 DEG C in this step, and drying time is 2h。
Step 5, it is put into box-type high-temperature furnace after the resulting green compact of above-mentioned drying being placed in silica crucible, first with 1~5 DEG C/rate of min from room temperature rises to 600 DEG C, 1h~3h is kept the temperature, then 900 DEG C is risen to the rate of 5 DEG C/min and keeps the temperature 2h, Last furnace cooling.
Embodiment 1
8.1589g basic magnesium carbonate, 7.7906g boric acid, 0.7975g polyvinyl alcohol is taken to be put into ball grinder.To ball grinder Middle addition 9ml deionized water, using wet ball grinding.Ball grinder is placed in the rate ball milling after planetary ball mill with 300r/min 8h obtains ceramic powder, the powder obtained after ball milling is placed in baking oven at 80 DEG C dry 15h, the powder after weighing drying Compression moulding in a mold, the equal 22mm of green compact diameter and thickness after molding, the green compact obtained after compacting are placed in 110 in baking oven DEG C dry 2h, is put into box-type high-temperature furnace, first with the rate of 2 DEG C/min after the green body after drying is then placed in the dry pot of quartz 600 DEG C are risen to from room temperature, 1h is kept the temperature, then rises to 900 DEG C with the rate of 5 DEG C/min and keep the temperature 2h, finally cool to room with the furnace Temperature.Sample after cooling is tested, measuring porosity is 62.57%, compression strength 10.32MPa.
Embodiment 2
8.1589g basic magnesium carbonate, 7.7906g boric acid, 0.1595g magnesium fluoride, 0.7975 g polyvinyl alcohol is taken to be put into ball In grinding jar.9ml deionized water is added into ball grinder, using wet ball grinding.By ball grinder be placed in after planetary ball mill with The rate ball milling 8h of 300r/min, obtains ceramic powder, the powder obtained after ball milling is placed in baking oven at 80 DEG C dry 15h, the powder compression moulding in a mold after weighing drying, green compact diameter and thickness after molding is 22mm, after compacting Obtained green compact are placed in 110 DEG C of dry 2h in baking oven, are put into box high temperature after the green body after drying is then placed in the dry pot of quartz In furnace, 600 DEG C are risen to from room temperature with the rate of 2 DEG C/min first, 1h is kept the temperature, then rises to 900 DEG C simultaneously with the rate of 5 DEG C/min 2h is kept the temperature, finally cools to room temperature with the furnace.Sample after cooling is tested, measuring porosity is 56.38%, compression strength For 13.82MPa.
Embodiment 3
8.1589g basic magnesium carbonate, 7.7906g boric acid, 0.4785g magnesium fluoride, 0.7975 g polyvinyl alcohol is taken to be put into ball In grinding jar.9ml deionized water is added into ball grinder, using wet ball grinding.By ball grinder be placed in after planetary ball mill with The rate ball milling 8h of 300r/min, obtains ceramic powder, the powder obtained after ball milling is placed in baking oven at 80 DEG C dry 15h, the powder compression moulding in a mold after weighing drying, green compact diameter and thickness after molding is 22mm, after compacting Obtained green compact are placed in 110 DEG C of dry 2h in baking oven, are put into box high temperature after the green body after drying is then placed in the dry pot of quartz In furnace, 600 DEG C are risen to from room temperature with the rate of 2 DEG C/min first, 1h is kept the temperature, then rises to 900 DEG C simultaneously with the rate of 5 DEG C/min 2h is kept the temperature, finally cools to room temperature with the furnace.Sample after cooling is tested, measuring porosity is 53.05%, compression strength For 14.43MPa.
Embodiment 4
8.1589g basic magnesium carbonate, 7.7906g boric acid, 0.7975g magnesium fluoride, 0.7975 g polyvinyl alcohol is taken to be put into ball In grinding jar.9ml deionized water is added into ball grinder, using wet ball grinding.By ball grinder be placed in after planetary ball mill with The rate ball milling 8h of 300r/min, obtains ceramic powder, the powder obtained after ball milling is placed in baking oven at 80 DEG C dry 15h, the powder compression moulding in a mold after weighing drying, green compact diameter and thickness after molding is 22mm, after compacting Obtained green compact are placed in 110 DEG C of dry 2h in baking oven, are put into box high temperature after the green body after drying is then placed in the dry pot of quartz In furnace, 600 DEG C are risen to from room temperature with the rate of 2 DEG C/min first, 1h is kept the temperature, then rises to 900 DEG C simultaneously with the rate of 5 DEG C/min 2h is kept the temperature, finally cools to room temperature with the furnace.Sample after cooling is tested, measuring porosity is 60.95%, compression strength For 14.09MPa.
In above-described embodiment 1-4, boric acid be it is commercially available, analyze it is pure;Basic magnesium carbonate, it is commercially available, it analyzes pure;Magnesium fluoride, it is commercially available, It analyzes pure;Polyvinyl alcohol, it is commercially available, it analyzes pure.
The performance and microstructure for the magnesium borate crystal whisker porous ceramics that the present invention produces are shown in Fig. 1-6.
The product of embodiment 1-4 is subjected to performance detection, the results are shown in Table one.
Table one

Claims (8)

1. a kind of preparation method of the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength, this method with Basic magnesium carbonate and boric acid are primary raw material, and magnesium fluoride is sintering aid, and polyvinyl alcohol is binder, and deionized water is solvent, The following steps are included:
1. weighing;
2. ball mill mixing;
3. 80 DEG C of dryings;
4. compression moulding;
5. 110 DEG C of dryings;
6. being sintered.
2. the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength according to claim 1 Preparation method, it is characterised in that: the basic magnesium carbonate that uses, boric acid by Mg:B molar ratio for 1: 1.1 ~ 1: 1.5 mixings, It is fluorinated the % of 1 % ~ 5 that content of magnesium is basic magnesium carbonate and boric acid gross mass, polyvinyl alcohol addition is basic magnesium carbonate and boron 5 % of sour gross mass, deionized water content are 55.56 % of basic magnesium carbonate and boric acid gross mass.
3. the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength according to claim 1 Preparation method, it is characterised in that: drum's speed of rotation is not less than 300 r/min during the ball mill mixing, and Ball-milling Time is 6 h ~10 h。
4. the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength according to claim 1 Preparation method, it is characterised in that: drying time is the h of 12 h ~ 15 in 80 DEG C of drying processes.
5. the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength according to claim 1 Preparation method, it is characterised in that: mixing quality is the g of 15 g ~ 20, the intensity of pressure 100 during the compression moulding MPa, forming diameter and height are 22 mm.
6. the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength according to claim 1 Preparation method, it is characterised in that: drying time is the h of 6 h ~ 10 in 110 DEG C of drying processes.
7. the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength according to claim 1 Preparation method, it is characterised in that: the sintering process is to be placed in the green body after drying after crucible to be put into the controllable height of program In temperature type resistance furnace, 600 DEG C are risen to from room temperature with the rate of 1 DEG C ~ 5 DEG C/min first, keeps the temperature the h of 1 h ~ 3, then 900 DEG C are risen to the rate of 5 DEG C/min and keep the temperature 2 h, last furnace cooling.
8. a kind of preparation method of the magnesium borate crystal whisker ceramic film support with suitable porosity and compression strength, feature exist In: the high compressive strength magnesium borate crystal whisker porous ceramic film support is using described in 1 ~ 7 any claim of patent requirements Method preparation.
CN201811450158.3A 2018-11-30 2018-11-30 A kind of preparation method with suitable porosity and compression strength magnesium borate crystal whisker ceramic film support Pending CN109456077A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877783A (en) * 2021-01-11 2021-06-01 东北大学 Method for preparing magnesium borate whisker by using magnesite

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877783A (en) * 2021-01-11 2021-06-01 东北大学 Method for preparing magnesium borate whisker by using magnesite
CN112877783B (en) * 2021-01-11 2022-04-01 东北大学 Method for preparing magnesium borate whisker by using magnesite

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