CN108623315A - A kind of preparation process of titanium alloy smelting oxidation yttrium powder - Google Patents
A kind of preparation process of titanium alloy smelting oxidation yttrium powder Download PDFInfo
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- CN108623315A CN108623315A CN201810412978.7A CN201810412978A CN108623315A CN 108623315 A CN108623315 A CN 108623315A CN 201810412978 A CN201810412978 A CN 201810412978A CN 108623315 A CN108623315 A CN 108623315A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
- C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
Abstract
The invention discloses a kind of titanium alloys to smelt the preparation process with oxidation yttrium powder, specifically includes following steps：（1）4N yttrium oxides are ground to certain fineness；（2）By step（1）Pelletizing is pressed into small-sized brick by the 4N yttrium oxides after grinding through mist projection granulating；（3）Brick is sintered in 1800 DEG C of high-temperature electric resistance furnaces, and held for some time；（4）Brick is broken into sand, then is ground into and requires grain size powder finished product；The present invention should preparation is simple, easily controllable, the yttrium oxide powder purity prepared is high, stable quality.
Description
Technical field
The invention belongs to powder preparation fields, and in particular to a kind of preparation process of titanium alloy smelting oxidation yttrium powder.
Background technology
With the needs of aerospace and many special trades, the application of titanium or titanium alloy is more and more extensive, but titanium and its
Alloy has particular/special requirement in smelting and casting to contacted refractory material, otherwise can make its small amounts and quality decline, warp
Smelting and casting that yttrium oxide material is particularly suitable for titanium or titanium alloy are studied, its oxidation will not be led to, but common yttrium oxide is logical
It crosses chemical method to be made, temperature is low when decomposing and calcining, is dissolved in acid, easily contact with water in air and hydration reaction occurs, and is indefinite
Shape powder, hole is more, can not use, and mainly uses electric smelting method production technology at present, i.e., after yttrium oxide being melted by electric arc furnaces,
Natural cooling recrystallizes, through crushing grinding at desired diameter of particle, the advantages of the technique：Y2O3Work is lost after high-temperature fusion
Property, it can more meet purposes requirement；Disadvantage：It is difficult to which graphite electrode in product is avoided to pollute, there are mass colour particulate matter, product yield to damage
Consumption；Therefore, it is urgently to be resolved hurrily as those skilled in the art to research and develop a kind of preparation process for the oxidation yttrium powder that can overcome drawbacks described above
The technical issues of.
Invention content
The technical problem to be solved by the present invention is to for the above disadvantage of the existing technology, propose a kind of titanium alloy
Smelt the preparation process with oxidation yttrium powder, should preparation is simple, easily controllable, the yttrium oxide powder purity prepared is high,
Stable quality.
The technical solution that the present invention solves the above technical problem is：
A kind of titanium alloy smelting preparation process of oxidation yttrium powder, specifically includes following steps：
（1）4N yttrium oxides are ground to certain fineness；
（2）By step（1）Pelletizing is pressed into small-sized brick by the 4N yttrium oxides after grinding through mist projection granulating；
（3）By step（2）Obtained brick is sintered in 1800 DEG C of high-temperature electric resistance furnaces, and keeps the temperature the 3-5h times；
（4）By step（3）Brick after sintering is broken into sand, then is ground into and requires grain size yttrium oxide powder finished product.
The technical solution that the present invention further limits is：
Further, aforementioned titanium alloy is smelted in the preparation process with oxidation yttrium powder, step（1）It is middle 4N yttrium oxides are ground to it is low
In 1 μm.
Aforementioned titanium alloy is smelted in the preparation process with oxidation yttrium powder, using yttrium oxide as raw material, is dissolved and is prepared with concentrated nitric acid
Carbon black is added in yttrium nitrate solution, stirs evenly by yttrium nitrate solution at room temperature, adds ammonium hydroxide, reacts 1-3h, is aged 1-
3d obtains the colloidal solution of black, continues to stir, and product is filtered, washed, is dried, is burnt in air atmosphere, keeps the temperature 2-
3h obtains the yttrium oxide of bulky grain, wherein：
Ammonium hydroxide is the ammonium hydroxide of 1.0mol/L, and drying temperature is 70-80 DEG C, and it is 900-1100 DEG C to burn temperature.
Technique effect, considered critical sedimentation time in the present invention, digestion time, because digestion time and calcination temperature are
The key of yttrium oxide is prepared, ageing is less than 4h, and precipitation particle is very thin, sad, more than ageing for 24 hours, obtains bulky grain precipitation, sternly
Severe control digestion time and calcination temperature, can prepare varying particle size, and particle is uniform, the bulky grain oxidation of good fluidity
Yttrium.
Technique effect, the present invention send preparation large-particle yttrium oxide using precipitation, prepare yttrium oxide powder both at home and abroad at present
Method it is very much, but sol-gel method is of high cost, and the period is long, low yield；Combustion method reaction is violent, is difficult to control；Spraying heat point
The reasons such as solution equipment investment is big, and the powder mobile phone of generation is more difficult, many preparation methods are also only limitted to laboratory research, and this
The charcoal of invention adsorbs ammonia water precipitating, and since carbon black is a kind of very strong adsorbent, it is heavy equably to absorb during the reaction
Starch, significantly reduces calcination degree when reunion degree of the particle in precipitation, separation, drying process and calcination, and
Burning phase generates the purity that gas does not interfere with powder.
Aforementioned titanium alloy is smelted in the preparation process with oxidation yttrium powder, step（2）Middle mist projection granulating is specially：
4N yttrium oxides, dispersant, binder, auxiliary agent after grinding is uniformly mixed, mixing is placed in ball grinder, then
Deionized water is added and ball milling ball is placed on ball mill, carries out ball mill mixing, mixed material is sent directly into sponging granulator
In, feed rate 4kg/h, sponging granulator inlet temperature is 300-320 DEG C, and control outlet temperature is 80-90 DEG C, through spraying
It is granulated, pelletizing is pressed into small-sized brick, wherein：
Auxiliary agent is counted in mass ratio：7-10%, dispersant 1-3%, binder：3-5%, surplus are the 4N yttrium oxides after grinding, above each
The sum of component is 100%.
Then technique effect is pressed into brick using mist projection granulating, pelletizing surface is regular, and smooth and texture is uniform, granularity
Distribution is in Unimodal Distribution, and biscuit density is high, can meet requirement.
Aforementioned titanium alloy is smelted in the preparation process with oxidation yttrium powder, ratio of grinding media to material, that is, ball milling ball and the 4N yttrium oxides after grinding
Weight ratio be 1-3:1, the ball mill mixing time is 5-7h, ball milling speed 200-300r/min.
Aforementioned titanium alloy is smelted in the preparation process with oxidation yttrium powder, and auxiliary agent is the mixture of aluminium oxide and yttrium oxide, is pressed
Mass ratio meter aluminium oxide：Yttrium oxide=4:3；Binder is polyvinyl alcohol；Dispersant is the ammonium citrate of equal proportion mixing and poly- second
Glycol.
The beneficial effects of the invention are as follows：
Mainly use electric smelting method production technology at present, i.e., after yttrium oxide being melted by electric arc furnaces, natural cooling recrystallization, through broken
Breakdown mill is at desired diameter of particle；Advantage：Y2O3It loses activity after high-temperature fusion, can more meet purposes requirement；Disadvantage：Very
Difficulty avoids graphite electrode in product from polluting, and has mass colour particulate matter, product yield lossy.
Step of the present invention（1）It is middle that 4N yttrium oxides are ground to certain fineness, it makes it easier to be sintered.
The present invention is pressed into after brick high temperature sintering again using that will aoxidize yttrium powder, and crushing grinding is cast at powder for titanium and its alloy
It makes；And process high-temperature sintering temperature is lost activity after yttrium oxide high temperature up to 1800 degree, more can combined use requirement, the present invention with
Traditional handicraft is compared：
1. product purity is high；
2. production process is easily controllable, stable quality.
Specific implementation mode
Embodiment 1
The present embodiment provides a kind of titanium alloys to smelt the preparation process with oxidation yttrium powder, specifically includes following steps：
A kind of titanium alloy smelting preparation process of oxidation yttrium powder, specifically includes following steps：
（1）4N yttrium oxides are ground to less than 1 μm；
（2）By step（1）Pelletizing is pressed into small-sized brick by the 4N yttrium oxides after grinding through mist projection granulating；
4N yttrium oxides, dispersant, binder, auxiliary agent after grinding is uniformly mixed, mixing is placed in ball grinder, then
Deionized water is added and ball milling ball is placed on ball mill, carries out ball mill mixing, mixed material is sent directly into sponging granulator
In, feed rate 4kg/h, sponging granulator inlet temperature is 310 DEG C, and control outlet temperature is 85 DEG C, will through mist projection granulating
Pelletizing is pressed into small-sized brick, wherein：
Auxiliary agent is counted in mass ratio：8%, dispersant 2%, binder：4%, surplus be grinding after 4N yttrium oxides, the above components it
Be 100%；
（3）By step（2）Obtained brick is sintered in 1800 DEG C of high-temperature electric resistance furnaces, and keeps the temperature the 4h times；
（4）By step（3）Brick after sintering is broken into sand, then is ground into and requires grain size yttrium oxide powder finished product.
In the present embodiment, yttrium oxide prepare it is specific as follows：
Using yttrium oxide as raw material, yttrium nitrate solution is prepared with concentrated nitric acid dissolving, carbon black is added in yttrium nitrate solution at room temperature,
It stirs evenly, adds ammonium hydroxide, react 2h, be aged 2d, obtain the colloidal solution of black, continue to stir, by product filtering, wash
It washs, dry, burnt in air atmosphere, keep the temperature 2.5h, obtain the yttrium oxide of bulky grain, wherein：
Ammonium hydroxide is the ammonium hydroxide of 1.0mol/L, and drying temperature is 75 DEG C, and it is 1000 DEG C to burn temperature.
In the present embodiment, step（3）The weight ratio of ratio of grinding media to material, that is, ball milling ball and the 4N yttrium oxides after grinding is 2:1, ball
Mill mixing time is 6h, ball milling speed 250r/min；Auxiliary agent is the mixture of aluminium oxide and yttrium oxide, meter oxidation in mass ratio
Aluminium：Yttrium oxide=4:3；Binder is polyvinyl alcohol；Dispersant is the ammonium citrate and polyethylene glycol of equal proportion mixing.This implementation
Example provides a kind of titanium alloy smelting preparation process of oxidation yttrium powder, specifically includes following steps：
Embodiment 2
A kind of titanium alloy smelting preparation process of oxidation yttrium powder, specifically includes following steps：
（1）4N yttrium oxides are ground to less than 1 μm；
（2）By step（1）Pelletizing is pressed into small-sized brick by the 4N yttrium oxides after grinding through mist projection granulating；
4N yttrium oxides, dispersant, binder, auxiliary agent after grinding is uniformly mixed, mixing is placed in ball grinder, then
Deionized water is added and ball milling ball is placed on ball mill, carries out ball mill mixing, mixed material is sent directly into sponging granulator
In, feed rate 4kg/h, sponging granulator inlet temperature is 320 DEG C, and control outlet temperature is 90 DEG C, will through mist projection granulating
Pelletizing is pressed into small-sized brick, wherein：
Auxiliary agent is counted in mass ratio：10%, dispersant 3%, binder：5%, surplus be grinding after 4N yttrium oxides, the above components it
Be 100%；
（3）By step（2）Obtained brick is sintered in 1800 DEG C of high-temperature electric resistance furnaces, and keeps the temperature the 5h times；
（4）By step（3）Brick after sintering is broken into sand, then is ground into and requires grain size yttrium oxide powder finished product.
In the present embodiment, yttrium oxide prepare it is specific as follows：
Using yttrium oxide as raw material, yttrium nitrate solution is prepared with concentrated nitric acid dissolving, carbon black is added in yttrium nitrate solution at room temperature,
It stirs evenly, adds ammonium hydroxide, react 3h, be aged 3d, obtain the colloidal solution of black, continue to stir, by product filtering, wash
It washs, dry, burnt in air atmosphere, keep the temperature 3h, obtain the yttrium oxide of bulky grain, wherein：
Ammonium hydroxide is the ammonium hydroxide of 1.0mol/L, and drying temperature is 80 DEG C, and it is 1100 DEG C to burn temperature.
In the present embodiment, step（3）The weight ratio of ratio of grinding media to material, that is, ball milling ball and the 4N yttrium oxides after grinding is 3:1, ball
Mill mixing time is 7h, ball milling speed 300r/min；Auxiliary agent is the mixture of aluminium oxide and yttrium oxide, meter oxidation in mass ratio
Aluminium：Yttrium oxide=4:3；Binder is polyvinyl alcohol；Dispersant is the ammonium citrate and polyethylene glycol of equal proportion mixing.
Embodiment 3
A kind of titanium alloy smelting preparation process of oxidation yttrium powder, specifically includes following steps：
（1）4N yttrium oxides are ground to less than 1 μm；
（2）By step（1）Pelletizing is pressed into small-sized brick by the 4N yttrium oxides after grinding through mist projection granulating；
4N yttrium oxides, dispersant, binder, auxiliary agent after grinding is uniformly mixed, mixing is placed in ball grinder, then
Deionized water is added and ball milling ball is placed on ball mill, carries out ball mill mixing, mixed material is sent directly into sponging granulator
In, feed rate 4kg/h, sponging granulator inlet temperature is 300 DEG C, and control outlet temperature is 80 DEG C, will through mist projection granulating
Pelletizing is pressed into small-sized brick, wherein：
Auxiliary agent is counted in mass ratio：7%, dispersant 1%, binder：3%, surplus be grinding after 4N yttrium oxides, the above components it
Be 100%；
（3）By step（2）Obtained brick is sintered in 1800 DEG C of high-temperature electric resistance furnaces, and keeps the temperature the 3h times；
（4）By step（3）Brick after sintering is broken into sand, then is ground into and requires grain size yttrium oxide powder finished product.
In the present embodiment, yttrium oxide prepare it is specific as follows：
Using yttrium oxide as raw material, yttrium nitrate solution is prepared with concentrated nitric acid dissolving, carbon black is added in yttrium nitrate solution at room temperature,
It stirs evenly, adds ammonium hydroxide, react 1h, be aged 1d, obtain the colloidal solution of black, continue to stir, by product filtering, wash
It washs, dry, burnt in air atmosphere, keep the temperature 2h, obtain the yttrium oxide of bulky grain, wherein：
Ammonium hydroxide is the ammonium hydroxide of 1.0mol/L, and drying temperature is 70 DEG C, and it is 900 DEG C to burn temperature.
In the present embodiment, step（3）The weight ratio of ratio of grinding media to material, that is, ball milling ball and the 4N yttrium oxides after grinding is 1:1, ball
Mill mixing time is 5h, ball milling speed 200r/min；Auxiliary agent is the mixture of aluminium oxide and yttrium oxide, meter oxidation in mass ratio
Aluminium：Yttrium oxide=4:3；Binder is polyvinyl alcohol；Dispersant is the ammonium citrate and polyethylene glycol of equal proportion mixing.
Titanium alloy using the present invention smelts the preparation process of use oxidation yttrium powder, and preparation is simple for this, is easy to control
System, the yttrium oxide powder purity prepared is high, stable quality.
In addition to the implementation, the present invention can also have other embodiment.It is all to use equivalent substitution or equivalent transformation shape
At technical solution, fall within the scope of protection required by the present invention.
Claims (6)
1. a kind of titanium alloy smelts the preparation process with oxidation yttrium powder, which is characterized in that specifically include following steps：
（1）4N yttrium oxides are ground to certain fineness；
（2）By step（1）Pelletizing is pressed into small-sized brick by the 4N yttrium oxides after grinding through mist projection granulating；
（3）By step（2）Obtained brick is sintered in 1800 DEG C of high-temperature electric resistance furnaces, and keeps the temperature the 3-5h times；
（4）By step（3）Brick after sintering is broken into sand, then is ground into and requires grain size yttrium oxide powder finished product.
2. titanium alloy according to claim 1 smelts the preparation process with oxidation yttrium powder, it is characterised in that：The step
（1）It is middle that 4N yttrium oxides are ground to less than 1 μm.
3. titanium alloy according to claim 1 smelts the preparation process with oxidation yttrium powder, it is characterised in that：The yttrium oxide
Prepare it is specific as follows：
Using yttrium oxide as raw material, yttrium nitrate solution is prepared with concentrated nitric acid dissolving, carbon black is added in yttrium nitrate solution at room temperature,
It stirs evenly, adds ammonium hydroxide, react 1-3h, be aged 1-3d, obtain the colloidal solution of black, continue to stir, product is filtered,
Washing, drying, burn in air atmosphere, keep the temperature 2-3h, obtain the yttrium oxide of bulky grain, wherein：
The ammonium hydroxide is the ammonium hydroxide of 1.0mol/L, and drying temperature is 70-80 DEG C, and it is 900-1100 DEG C to burn temperature.
4. titanium alloy according to claim 1 smelts the preparation process with oxidation yttrium powder, it is characterised in that：Step（2）In
The mist projection granulating is specially：
4N yttrium oxides, dispersant, binder, auxiliary agent after grinding is uniformly mixed, mixing is placed in ball grinder, then
Deionized water is added and ball milling ball is placed on ball mill, carries out ball mill mixing, mixed material is sent directly into sponging granulator
In, feed rate 4kg/h, sponging granulator inlet temperature is 300-320 DEG C, and control outlet temperature is 80-90 DEG C, through spraying
It is granulated, pelletizing is pressed into small-sized brick, wherein：
Auxiliary agent is counted in mass ratio：7-10%, dispersant 1-3%, binder：3-5%, surplus are the 4N yttrium oxides after grinding, above each
The sum of component is 100%.
5. titanium alloy according to claim 4 smelts the preparation process with oxidation yttrium powder, it is characterised in that：Ratio of grinding media to material, that is, ball
The weight ratio of abrading-ball and the 4N yttrium oxides after grinding is 1-3:1, the ball mill mixing time is 5-7h, ball milling speed 200-300r/
min。
6. titanium alloy according to claim 4 smelts the preparation process with oxidation yttrium powder, it is characterised in that：The auxiliary agent
For the mixture of aluminium oxide and yttrium oxide, aluminium oxide is counted in mass ratio：Yttrium oxide=4:3；The binder is polyvinyl alcohol；Institute
State the ammonium citrate and polyethylene glycol that dispersant is equal proportion mixing.
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