CN100453505C - Method for preparing low-expansion aluminium titanates ceramic catheter - Google Patents
Method for preparing low-expansion aluminium titanates ceramic catheter Download PDFInfo
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- CN100453505C CN100453505C CNB2006100698606A CN200610069860A CN100453505C CN 100453505 C CN100453505 C CN 100453505C CN B2006100698606 A CNB2006100698606 A CN B2006100698606A CN 200610069860 A CN200610069860 A CN 200610069860A CN 100453505 C CN100453505 C CN 100453505C
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Abstract
The invention relates to a preparation method of a low expansion alumina titanate ceramics delivery tube. Firstly, alumina titanate ceramics is composed, made into powder, gel cast and heated, thus the alumina titanate ceramics delivery tube is obtained. The weight percentages composition of composite materials of the alumina titanate ceramics are that: 31.78 to 53.1 percent of alumina, 32.82 to 46.9 percent of titanium dioxide and 0 to 30 percent of additive zero to thirty percent, wherein the weight compositions of the additive are that: 0 to 30 percent of porzite, 0 to 30 percent of magnesia-alumina spinel, 0 to 40 percent of dichroite and 0 to 100 percent of light magnesium carbonate. The alumina titanate ceramics delivery tube made of the completely novel ingredients has a small thermal expansion coefficient, good thermal stability can meet using needs. The gel-casting method adopted is simple in process, convenient in operation, short in production period, small in working amount and thermal expansion coefficient, high in working efficiency, high in green strength, high in rate of finished products and good in product performance, even in microstructure tissue, good in thermal stability, high in precision of product matched size, and is suitable for the production of products with complicated shape and large size and is particularly suited to manufacturing production.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium titanates ceramic catheter, belong to the special cermacis preparing technical field.
Background technology
Aluminium titanates ceramic catheter is the ceramic component that uses in the aluminium alloy press injector, and its effect is that aluminium alloy melt is transported in the mould of aluminium alloy press injector by aluminium titanates ceramic catheter.Because aluminium alloy melt is frequently travelled to and fro between ceramic catheter during the work of aluminium alloy press injector, requires ceramic catheter can stand violent thermal shocking, thermal expansivity is little, Heat stability is good.
Because batching and the many-sided influence of preparation technology, existing aluminium titanates ceramic catheter can't satisfy this requirement well, existing forming method has multiple, more employing be isostatic pressing method and filling forming method, shortcoming such as isostatic pressing method exists that facility investment is big, complex process, labour intensity are big; There are shortcomings such as the product microstructure is inhomogeneous, poor reliability, product coordinating size low precision in filling forming method.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of low-expansion aluminium titanates ceramic catheter, brand-new batching is formed, and adopts the type method of congealing into of annotating, technology is simple, and is easy to operate, with short production cycle, the work workload is little, the production efficiency height, green strength height, the rate that manufactures a finished product height, product performance are superior, the microstructure homogeneous microstructure, thermal expansivity is little, Heat stability is good.
The preparation method of low-expansion aluminium titanates ceramic catheter of the present invention, at first synthetic alumina titanate ceramics, make powder after, annotate the type that congeals into, burn till at last and make, the weight percent of the synthesis material of alumina titanate ceramics consists of:
Aluminium sesquioxide 37.18～53.1%, titanium dioxide 32.82～46.9% and additive 0～30%; Wherein, the weight of additive consists of: mullite 0～30%, magnesium-aluminium spinel 0～30%, trichroite 0～40% and magnesium basic carbonate 0～100%.
Alumina titanate ceramics powder synthetic suitable condition: oxidizing atmosphere, 1200～1550 ℃ of synthesis temperatures.The synthetic alumina titanate ceramics reaches particle diameter below 3 μ m through fineness behind the ball milling, and it is standby to get the alumina titanate ceramics powder.
The alumina titanate ceramics powder joined to make in the organic solution annotate the type slurry that congeals into, wherein, the weight percent of organic solution consists of: organic monomer 0.5～70% and distilled water 30～99.5%, organic monomer is by acrylamide and N, and N-methylene radical acrylamide is according to weight ratio 10: the mixed of (0.1～4) is made.
The pH value of organic solution is controlled to be 9～10 and suits.
Among the present invention:
The congeal into weight percent of type slurry of notes consists of: alumina titanate ceramics powder 40～90%, organic solution 10～35%, dispersion agent 0～25%.
Wherein, dispersion agent is that weight concentration is 20～60% polyacrylic acid ammonium solution; Use pH value to adjust the pH value that organic solution is adjusted in agent, it is acid solution or alkali lye that pH value is adjusted agent, is the lactic acid of 40～60% ammoniacal liquor or 40～60% or 40～60% hydrochloric acid etc. as weight concentration, and add-on is as the criterion with the pH value requirement of satisfied adjustment.
The same with the common notes type method of congealing into, to annotate the type slurry that congeals into and preferably handle and eliminate bubble through vacuum exhaust, the vacuum tightness of vacuum-treat control is generally-0.08～-0.1MPa.
Add weight concentration in the moulding slurry after vacuum exhaust and be 0.1～5% ammonium persulfate solution as initiator, promote the gelling moulding, add-on is generally 0.1～5% of slurry volume.
The adding weight concentration is the N greater than 98% when adding initiator, and N, N, N, Tetramethyl Ethylene Diamine solution can accelerate to annotate the type process of congealing into as catalyzer, and add-on is generally slurry volume 0～5%.After fully stirring, the barrel moulding of the centrifugal notes of the direct injection of moulding slurry being coagulated shaper gets final product.
Other notes coagulate operation to be annotated the type that congeals into according to routine and requires to get final product, as the demoulding, drying, mold temperature, time etc.
With the later half product of moulding in oxidizing atmosphere, under 1300～1600 ℃ temperature, burn till product, obtain finished product through follow-up arrangement processing.
Raw materials used equal market is on sale among the present invention, can directly buy, and main raw material purity is technical pure.
Aluminium sesquioxide adopt purity be more than 99.5%, median size is less than industrial α-Al of 2 μ m
2O
3Powder.
Titanium dioxide adopt purity be 98% or more, median size is less than the industrial TiO of the rutile-type of 1 μ m
2Powder.
Mullite adopt purity be more than 95%, median size is less than the industrial mullite synthesizing powder of 2 μ m.
Magnesium-aluminium spinel adopt purity be more than 95%, median size is less than the industrial synthetic MgAl spinal powder of 2 μ m.
Trichroite adopt purity be 95% or more, median size is less than the industrial powder of the synthesis of dichroite of 2 μ m.
Magnesium basic carbonate employing content of magnesia is the industrial magnesium basic carbonate powder more than 40%.
The aluminium titanates ceramic catheter technical indicator of preparation method's gained of the present invention is as follows:
The thermal expansivity of alumina titanate ceramics is: 0～0.8 * 10
-6/ ℃
The bending strength of alumina titanate ceramics is 30～60MPa.
The preparation method of low-expansion aluminium titanates ceramic catheter of the present invention, brand-new batching is formed, and the aluminium titanates ceramic catheter thermal expansivity of gained is little, and Heat stability is good satisfies service requirements.Adopt and annotate the type method of congealing into, technology is simple, and is easy to operate, with short production cycle, the work workload is little, the production efficiency height, the green strength height, the rate that manufactures a finished product height, product performance are superior, the microstructure homogeneous microstructure, thermal expansivity is little, and Heat stability is good is fit to preparation complicated shape, large size product, product coordinating size precision height, the special big production of suitability for industrialized.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
The ingredients by weight percentage composition of synthetic alumina titanate ceramics is:
Aluminium sesquioxide 48%, titanium dioxide 41% and additive 11%, wherein, the weight of additive consists of: magnesium-aluminium spinel 18%, magnesium basic carbonate 64%, trichroite 9%, mullite 9%.
Above-mentioned powder is mixed, mix back synthetic alumina titanate ceramics under 1320 ℃ temperature, ball milling gets the alumina titanate ceramics powder to granularity (being maximum particle diameter 3 μ m) below 3 μ m, and is standby.
The weight percent of organic solution consists of:
Organic monomer 12%, distilled water 88%, wherein the weight of organic monomer consists of N, N-methylene radical acrylamide 2%, acrylamide 98%;
During the moulding slurry weight is formed, alumina titanate ceramics powder 87%, organic solution 12.3%, dispersion agent: 0.7% is prepared into the alumina titanate ceramics slurry in ball mill.
Dispersion agent employing weight concentration is 30% polyacrylic acid ammonium solution;
PH value adjustment agent employing weight concentration is 40% ammoniacal liquor, and the pH value that is adjusted to organic solution is 9.5;
With weight concentration is that 2% ammonium persulfate solution is as initiator.
Moulding and burning till:
With alumina titanate ceramics moulding slurry, vacuum-treat control vacuum tightness reaches-0.1MPa, do not have bubble to overflow to the slurry till, fully stir after adding the initiator of slurry volume 1%, the time was controlled in 3 minutes, as 2 minutes.Then the moulding slurry is injected the barrel that centrifugal notes coagulate shaper and carry out moulding, 90 ℃ of temperature, 15 minutes time, cure and demold, the base substrate after will drying at last burns till under 1350 ℃ temperature, makes aluminium titanates low expansion ceramic catheter of the present invention.
Embodiment 2
The ingredients by weight percentage composition of synthetic alumina titanate ceramics is:
Aluminium sesquioxide 47.0%, titanium dioxide 43.0% and additive 10%, wherein, additive is a magnesium basic carbonate.
Above-mentioned powder is mixed, mixes back synthetic alumina titanate ceramics under 1460 ℃ temperature, ball milling to granularity below 3 μ m, the alumina titanate ceramics powder, standby.
The weight percent of organic solution consists of:
Organic monomer 5%, distilled water 95%, wherein the weight of organic monomer consists of N, N-methylene radical acrylamide 3%, acrylamide 97%;
During the moulding slurry weight is formed, alumina titanate ceramics powder 87%, organic solution 12.4%, dispersion agent: 0.6%; In ball mill, be prepared into the alumina titanate ceramics slurry.
Dispersion agent adopts the polyacrylic acid ammonium solution, and weight concentration is 40%;
PH value adjustment agent employing weight concentration is 40% ammoniacal liquor, and the pH value that is adjusted to organic solution is 9.3;
Initiator employing weight concentration is 4% ammonium persulfate solution.
Moulding and burning till:
With alumina titanate ceramics moulding slurry, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having to the slurry bubble to overflow, fully stir 2.5 minutes time after adding the initiator of slurry volume 0.1%, then the moulding slurry is injected the barrel that centrifugal notes coagulate shaper, 90 ℃ of temperature, 20 minutes time, curing and demolding, base substrate after will drying at last burns till under 1520 ℃ temperature, makes aluminium titanates low expansion ceramic catheter of the present invention.
The ingredients by weight percentage composition of embodiment 3, synthetic alumina titanate ceramics is:
Aluminium sesquioxide 53%, titanium dioxide 42% and additive 5% are formed, and additive is a trichroite.
Above-mentioned powder is mixed, synthetic alumina titanate ceramics under 1350 ℃ temperature, ball milling to granularity below 3 μ m, the alumina titanate ceramics powder, standby.
Organic solution weight percent consist of:
Organic monomer 40%, distilled water 6%, wherein the weight of organic monomer consists of N, N-methylene radical acrylamide 1%, acrylamide 99%;
During the moulding slurry weight is formed, alumina titanate ceramics powder 82%, organic solution 17.8%, dispersion agent: 0.2%, in ball mill, be prepared into the alumina titanate ceramics slurry.
Dispersion agent adopts the polyacrylic acid ammonium solution, and weight concentration is 50%;
PH value adjustment agent employing weight concentration is 40% ammoniacal liquor, and the pH value that is adjusted to organic solution is 9.8;
Initiator employing weight concentration is 3% ammonium persulfate solution;
Catalyzer employing weight concentration is the N greater than 98%, N, N, N, Tetramethyl Ethylene Diamine solution (the directly reagent product of Gou Maiing).
Moulding and burning till:
With alumina titanate ceramics moulding slurry, vacuum-treat to vacuum tightness reaches-0.08MPa, till not having to the slurry bubble to overflow, fully stir after adding the initiator of slurry volume 4% and 3% catalyzer, 2 minutes time, then the moulding slurry is injected the barrel that centrifugal notes coagulate shaper, 90 ℃ of temperature, 16 minutes time, curing and demolding; Base substrate after will drying at last burns till under 1550 ℃ temperature, makes aluminium titanates low expansion ceramic catheter of the present invention.
The ingredients by weight percentage composition of embodiment 4, synthetic alumina titanate ceramics is:
Aluminium sesquioxide 42%, titanium dioxide 33% and additive 25% are formed, and wherein, the weight of additive consists of: magnesium basic carbonate 55%, magnesium-aluminium spinel 20%, trichroite 15%, mullite 10%.
Above-mentioned powder is mixed, synthetic alumina titanate ceramics under 1320 ℃ temperature, ball milling to granularity below 3 μ m, the alumina titanate ceramics powder, standby.
Organic solution weight percent consist of:
Organic monomer 40%, distilled water 60%, wherein the weight of organic monomer consists of N, N-methylene radical acrylamide 1%, acrylamide 99%;
During the moulding slurry weight is formed, alumina titanate ceramics powder 70%, organic solution 29%, dispersion agent: 1%, in ball mill, be prepared into the alumina titanate ceramics slurry.
Dispersion agent adopts the polyacrylic acid ammonium solution, and weight concentration is 60%;
PH value adjustment agent employing weight concentration is 40% ammoniacal liquor, and the pH value that is adjusted to organic solution is 9.6;
Initiator employing weight concentration is 4% ammonium persulfate solution.
Moulding and burning till:
With alumina titanate ceramics moulding slurry, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having to the slurry bubble to overflow, fully stir after adding the initiator of slurry volume 2%, 2 minutes time, then the moulding slurry is injected the barrel that centrifugal notes coagulate shaper, 90 ℃ of temperature, 16 minutes time, curing and demolding; Base substrate after will drying at last burns till under 1400 ℃ temperature, makes aluminium titanates low expansion ceramic catheter of the present invention.
The ingredients by weight percentage composition of embodiment 5, synthetic alumina titanate ceramics is:
Aluminium sesquioxide 50%, titanium dioxide 45% and additive 5% are formed, and wherein, the weight of additive consists of: magnesium basic carbonate 50%, magnesium-aluminium spinel 20%, trichroite 20%, mullite 10%.
Above-mentioned powder is mixed, synthetic alumina titanate ceramics under 1320 ℃ temperature, ball milling to granularity below 3 μ m, the alumina titanate ceramics powder, standby.
Organic solution weight percent consist of:
Organic monomer 40%, distilled water 60%, wherein the weight of organic monomer consists of N, N-methylene radical acrylamide 4%, acrylamide 96%;
During the moulding slurry weight is formed, alumina titanate ceramics powder 70%, organic solution 29%, dispersion agent: 1%, in ball mill, be prepared into the alumina titanate ceramics slurry.
Dispersion agent adopts the polyacrylic acid ammonium solution, and weight concentration is 45%;
PH value adjustment agent employing weight concentration is 50% ammoniacal liquor, and the pH value that is adjusted to organic solution is 9.6;
Initiator employing weight concentration is 3.5% ammonium persulfate solution.
Moulding and burning till:
With alumina titanate ceramics moulding slurry, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having to the slurry bubble to overflow, fully stir after adding the initiator of slurry volume 4%, 1.5 minutes time, then the moulding slurry is injected the barrel that centrifugal notes coagulate shaper, 93 ℃ of temperature, 18 minutes time, curing and demolding; Base substrate after will drying at last burns till under 1530 ℃ temperature, makes aluminium titanates low expansion ceramic catheter of the present invention.
The ingredients by weight percentage composition of embodiment 6, synthetic alumina titanate ceramics is:
Aluminium sesquioxide 45%, titanium dioxide 35% and additive 20% are formed, and wherein, the weight of additive consists of: magnesium basic carbonate 70%, magnesium-aluminium spinel 15%, trichroite 10%, mullite 5%.
Above-mentioned powder is mixed, synthetic alumina titanate ceramics under 1300 ℃ temperature, ball milling to granularity below 3 μ m, the alumina titanate ceramics powder, standby.
Organic solution weight percent consist of:
Organic monomer 50%, distilled water 50%, wherein the weight of organic monomer consists of N, N-methylene radical acrylamide 1%, acrylamide 99%;
During the moulding slurry weight is formed, alumina titanate ceramics powder 60%, organic solution 35%, dispersion agent: 5%, in ball mill, be prepared into the alumina titanate ceramics slurry.
Dispersion agent adopts the polyacrylic acid ammonium solution, and weight concentration is 35%;
PH value adjustment agent employing weight concentration is 55% ammoniacal liquor, and the pH value that is adjusted to organic solution is 9.6;
Initiator employing weight concentration is 3% ammonium persulfate solution.
Moulding and burning till:
With alumina titanate ceramics moulding slurry, vacuum-treat to vacuum tightness reaches-0.1MPa, till not having to the slurry bubble to overflow, fully stir after adding the initiator of slurry volume 3%, 2.5 minutes time, then the moulding slurry is injected the barrel that centrifugal notes coagulate shaper, 78 ℃ of temperature, 22 minutes time, curing and demolding; Base substrate after will drying at last burns till under 1450 ℃ temperature, makes aluminium titanates low expansion ceramic catheter of the present invention.
Claims (9)
1, a kind of preparation method of low-expansion aluminium titanates ceramic catheter is characterized in that at first synthetic alumina titanate ceramics, make powder after, annotate the type that congeals into, burn till at last and make, the weight percent of the synthesis material of alumina titanate ceramics consists of:
Aluminium sesquioxide 37.18～53.1%, titanium dioxide 32.82～46.9% and additive 0～30%; Wherein, the weight of additive consists of: mullite 0～30%, magnesium-aluminium spinel 0～30%, trichroite 0～40% and magnesium basic carbonate 0～100%;
The alumina titanate ceramics powder joined to make in the organic solution annotate the type slurry that congeals into, wherein, the weight percent of organic solution consists of: organic monomer 0.5～70% and distilled water 30～99.5%, organic monomer is by acrylamide and N, and N-methylene radical acrylamide is according to weight ratio 10: the mixed of (0.1～4) is made.
2, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 1 is characterized in that alumina titanate ceramics is synthetic under 1200～1550 ℃ temperature in oxidizing atmosphere.
3, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 1 is characterized in that the pH value of organic solution is controlled to be 9～10.
4, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 3 is characterized in that annotating the congeal into weight percent of type slurry and consists of: alumina titanate ceramics powder 40～90%, organic solution 10～35%, dispersion agent 0～25%.
5, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 4 is characterized in that dispersion agent is that weight concentration is 20～60% polyacrylic acid ammonium solution.
6,, it is characterized in that annotating and congeal into the type slurry through vacuum exhaust processing elimination bubble according to the preparation method of the described low-expansion aluminium titanates ceramic catheter of the arbitrary claim of claim 1-5.
7, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 6 is characterized in that in the moulding slurry after vacuum exhaust adding weight concentration and is 0.1～5% ammonium persulfate solution as initiator.
8, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 7, it is characterized in that when adding initiator, adding weight concentration for greater than 98%% N, N, N, N, Tetramethyl Ethylene Diamine solution is as catalyzer, after fully stirring, the moulding slurry injected the barrel that centrifugal notes coagulate shaper carry out moulding.
9, the preparation method of low-expansion aluminium titanates ceramic catheter according to claim 8 is characterized in that the later half product of moulding is burnt till under 1300～1600 ℃ temperature in oxidizing atmosphere.
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|---|---|---|---|
| CNB2006100698606A CN100453505C (en) | 2006-08-03 | 2006-08-03 | Method for preparing low-expansion aluminium titanates ceramic catheter |
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|---|---|---|---|
| CNB2006100698606A CN100453505C (en) | 2006-08-03 | 2006-08-03 | Method for preparing low-expansion aluminium titanates ceramic catheter |
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|---|---|
| CN101117287A CN101117287A (en) | 2008-02-06 |
| CN100453505C true CN100453505C (en) | 2009-01-21 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108484161B (en) * | 2018-06-20 | 2020-11-03 | 上海定向材料科技有限公司 | Aluminum titanate composite material and preparation method thereof |
| CN108649148B (en) * | 2018-06-20 | 2021-05-14 | 上海定向材料科技有限公司 | Preparation method of barren aluminum titanate composite material sagger |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081394A (en) * | 1992-07-15 | 1994-02-02 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Gradient creamics with ceramic membrane fenestrata |
| CN1483561A (en) * | 2002-09-17 | 2004-03-24 | 山东中博先进材料股份有限公司 | Method for preparing thin wall ceramic pipe and centrifugal formation machine |
-
2006
- 2006-08-03 CN CNB2006100698606A patent/CN100453505C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081394A (en) * | 1992-07-15 | 1994-02-02 | 国家建筑材料工业局山东工业陶瓷研究设计院 | Gradient creamics with ceramic membrane fenestrata |
| CN1483561A (en) * | 2002-09-17 | 2004-03-24 | 山东中博先进材料股份有限公司 | Method for preparing thin wall ceramic pipe and centrifugal formation machine |
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