CN109627005A - A method of calcirm-fluoride crystalline ceramics is prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride - Google Patents
A method of calcirm-fluoride crystalline ceramics is prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride Download PDFInfo
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- CN109627005A CN109627005A CN201811564702.7A CN201811564702A CN109627005A CN 109627005 A CN109627005 A CN 109627005A CN 201811564702 A CN201811564702 A CN 201811564702A CN 109627005 A CN109627005 A CN 109627005A
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- C04B35/515—Shaped 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
- C04B35/553—Shaped 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 fluorides
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/645—Pressure sintering
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Abstract
The invention discloses a kind of methods for preparing calcirm-fluoride crystalline ceramics as the vacuum heating-press sintering of auxiliary agent using lithium fluoride, comprising the following steps: 1) preparation of powder raw material；2) sample is filled；3) sintering of crystalline ceramics；4) processing of ceramics sample to get arrive calcirm-fluoride crystalline ceramics.Present invention has an advantage that using ultrasonic disperse to mixed-powder, mix well calcirm-fluoride with fluorination lithium powder, during the sintering process, added lithium fluoride can promote the densification process of calcirm-fluoride powder, conducive to the preparation of calcirm-fluoride crystalline ceramics.Present invention optimizes the preparation processes of calcirm-fluoride crystalline ceramics.The calcirm-fluoride crystalline ceramics that the present invention prepares has good transparency.
Description
Technical field
The present invention relates to fluoride crystalline ceramics preparation fields, and specially one kind is using commercially available calcirm-fluoride powder as raw material, fluorine
Change lithium is auxiliary agent, the method for preparing crystalline ceramics by vacuum heating-press sintering.
Background technique
Calcirm-fluoride (CaF2) with transmitance is high, refractive index is low, transmission peak wavelength range is wide and the superiority such as phonon energy is low
Can, it is widely paid close attention to as optical material.Crystalline ceramics as a kind of novel optical material, not only have high temperature resistant,
The advantages that corrosion-resistant and high-intensitive, there is not yet the cleavage surface in monocrystalline, and preparation process is also simpler compared to monocrystalline, tool
Have broad application prospects.In recent years, the excellent calcirm-fluoride crystalline ceramics of exploitation processability becomes a big research hotspot.Mesh
Before, preparing calcirm-fluoride crystalline ceramics mainly includes using calcirm-fluoride powder and using calcium fluoride mono crystal as two big approach of raw material.
It is being prepared in calcirm-fluoride crystalline ceramics technique using powder as raw material, the raw materials used fluorination mainly synthesized with chemical method
Based on calcium powder.Synthesize calcirm-fluoride powder complexity crystalline ceramics preparation flow by chemical method has researcher to pass through in recent years
With discharge plasma sintering technology (SPS), crystalline ceramics directly is prepared (referring to document F by raw material of commercially available calcirm-fluoride powder
Nakamura, T Kato, G Okada, et al. Scintillation and dosimeter properties of
CaF2 transparent ceramics doped with Nd3+ produced by SPS, J. Eur. Ceram. Soc.
37 (2017) 4919-4924).Process of this technique without chemical method synthesis calcirm-fluoride powder, but the ceramics sample prepared is variable
Black, optical quality is lower.There is researcher to be separated powder raw material and graphite jig with one layer of refractory metal foil again, passes through electric discharge
Plasma sintering prepares the good calcium fluoride ceramic of transparency (referring to document P Wang, M Yang, S Zhang, et
al. Suppression of carbon contamination in SPSed CaF2 transparent ceramics by
37 (2017) 4103-4107 of Mo foil, J. Eur. Ceram. Soc.), but the crystalline ceramics prepared is easy to crack.Heat
Pressure sintering is to prepare the most commonly used sintering technology of calcirm-fluoride crystalline ceramics at present, is sintered compared to discharge plasma, institute
Need equipment simple, it is easy to operate.However, commercially available calcirm-fluoride powder is more much lower than the powder sintered activity that chemical method synthesizes, pass through
The calcium fluoride ceramic that vacuum heating-press sintering is prepared is completely opaque (referring to document W Li, H Huang, B Mei, et al.
Comparison of commercial and synthesized CaF2 powders for preparing
43 (2017) 10403-10409 of transparent ceramics, Ceram. Int.).
It is well known that often selecting suitable sintering aid in crystalline ceramics sintering process, promote the densification of powder
Journey, and reduce sintering temperature.Lithium fluoride, chemical formula LiF, about 840 DEG C of fusing point, CaF2The eutectic point temperature of-LiF system is only
There are 769 DEG C, and the ionic radius between Li and Ca differs larger.In calcirm-fluoride crystalline ceramics sintering process, lithium fluoride is selected
For auxiliary agent, conducive to the densification process for promoting calcirm-fluoride powder.
Therefore, one kind is developed using commercially available calcirm-fluoride powder as raw material, and lithium fluoride is auxiliary agent, is prepared by vacuum heating-press sintering
The method of calcirm-fluoride crystalline ceramics optimizes existing crystalline ceramics preparation process, has great importance.
Summary of the invention
To solve deficiency in the prior art, the present invention provides one kind using lithium fluoride as auxiliary agent, commercially available calcirm-fluoride powder
For raw material, the method that calcirm-fluoride crystalline ceramics is prepared by vacuum hot pressing sintering technique.
The object of the present invention is achieved like this:
A method of calcirm-fluoride crystalline ceramics being prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride, key step includes powder
The preparation of raw material and the sintering of crystalline ceramics, specific steps include:
1) preparation of powder raw material: weighing the setting commercially available calcirm-fluoride powder of quality, adds appropriate fluorination lithium powder, anhydrous second is added
Alcohol through ultrasonic disperse, is mixed, is dried for standby；
2) it fills sample: mixed-powder being fitted into graphite jig, and is separated mold and powder with graphite paper；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove and is sintered；
4) processing of ceramics sample: taking out ceramics after sintering, is processed by shot blasting sample to get transparent to calcirm-fluoride
Ceramics.
Calcirm-fluoride used is commercially available with fluorination lithium powder in the step 1), wherein calcirm-fluoride purity >=99%, fluorination
Lithium purity >=99.5%；
In the step 1) calcirm-fluoride and lithium fluoride mixed-powder, the content for adding fluorination lithium powder is 0.2wt%-
2.0wt%；
Step 1) the ultrasonic disperse time is 20min-60min；
Sintering method is vacuum heating-press sintering in the step 3), and sintering temperature is 700 DEG C -900 DEG C, and vacuum degree is better than
10Pa, pressure 30MPa-50MPa, soaking time 3h-8h.
Positive beneficial effect: for the present invention using lithium fluoride as auxiliary agent, commercially available calcirm-fluoride powder is raw material, is burnt by vacuum hotpressing
Knot prepares calcirm-fluoride crystalline ceramics.Ultrasonic disperse is used to mixed-powder raw material, mixes calcirm-fluoride more with fluorination lithium powder
Uniformly, during the sintering process, added lithium fluoride can promote the densification process of calcirm-fluoride powder, and it is transparent to be conducive to calcirm-fluoride
The preparation of ceramics.The calcirm-fluoride crystalline ceramics that the present invention prepares has good transparency.
Detailed description of the invention
Fig. 1 is commercially available calcirm-fluoride powder picture used in the present invention (800 times of amplification)；
Fig. 2 is picture (amplification 50000 times) of the commercially available calcirm-fluoride powder used in the present invention after ultrasonic disperse；
Fig. 3 is lithium fluoride powder picture used in the present invention (5000 times of amplification)；
Fig. 4 is the calcirm-fluoride crystalline ceramics picture prepared at 800 DEG C.
Specific embodiment
In order to better understand the present invention, with reference to the accompanying drawing, preferred embodiment is described in detail, but should not be with this
It limits the scope of the invention.On the contrary, providing these examples is to explain and illustrate basic principle and reality of the invention
Using to enable others skilled in the art to understand the present invention and make specific expected modification.If without especially saying
Bright, the various raw materials and other consumptive materials used in the present invention can be commercially available by market.
Embodiment 1
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content of lithium fluoride
2.0wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 60min, then
It mixes well, is put into baking oven and is dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 800 DEG C, then apply pressure 30MPa, keeps the temperature 3h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 800 DEG C.
If Fig. 1 is commercially available calcirm-fluoride powder picture used in the present invention (800 times of amplification), powder raw material is agglomerated into partial size and is
Tens microns of bulky grain.Fig. 2 is picture (amplification 50000 of the commercially available calcirm-fluoride powder used in the present invention after ultrasonic disperse
Times), it can be seen that the bulky grain in Fig. 1 is through ultrasonic disperse at the little particle of nano-scale.Fig. 3 is lithium fluoride used in the present invention
Powder picture (5000 times of amplification), partial size is not more than 20 μm.Fig. 4 is the calcirm-fluoride crystalline ceramics figure prepared at 800 DEG C
Piece, ceramics have good transparency.
Embodiment 2
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content of lithium fluoride
2.0wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 60 min, so
After mix well, be put into baking oven and be dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 700 DEG C, then apply pressure 30MPa, keeps the temperature 3h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 700 DEG C.
Embodiment 3
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content of lithium fluoride
2.0wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 20min, then
It mixes well, is put into baking oven and is dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 730 DEG C, then apply pressure 50MPa, keeps the temperature 3h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 730 DEG C.
Embodiment 4
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content of lithium fluoride
0.2wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 60min, then
It mixes well, is put into baking oven and is dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 900 DEG C, then apply pressure 30MPa, keeps the temperature 8h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 900 DEG C.
Embodiment 5
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content of lithium fluoride
0.5wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 30min, then fill
Divide and mix, is put into baking oven and is dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 850 DEG C, then apply pressure 50MPa, keeps the temperature 5h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 850 DEG C.
Embodiment 6
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content 1.0 of lithium fluoride
Wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 50min, then sufficiently
It mixes, is put into baking oven and is dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 750 DEG C, then apply pressure 50MPa, keeps the temperature 5h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 750 DEG C.
Embodiment 7
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, and addition fluorination lithium powder makes the content of lithium fluoride
1.0wt% is added dehydrated alcohol, so that dehydrated alcohol is flooded powder, be placed in ultrasonic cleaner and be ultrasonically treated 40min, then fill
Divide and mix, is put into baking oven and is dried for standby；
2) it fills sample: weighing the mixed-powder that 2g step 1) obtains, be fitted into the graphite jig that internal diameter is 16 mm, and use graphite paper
Mold and mixed-powder are separated；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, heating
To 700 DEG C, then apply pressure 50MPa, keeps the temperature 8h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then with polishing machine to sample
It is processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 700 DEG C.
For the present invention using lithium fluoride as auxiliary agent, commercially available calcirm-fluoride powder is raw material, prepares calcirm-fluoride by vacuum heating-press sintering
Crystalline ceramics.Ultrasonic disperse is used to mixed-powder raw material, mixes calcirm-fluoride with fluorination lithium powder more uniform, sintered
Cheng Zhong, added lithium fluoride can promote the densification process of calcirm-fluoride powder, conducive to the preparation of calcirm-fluoride crystalline ceramics.This
Inventing the calcirm-fluoride crystalline ceramics prepared has good transparency.
It should finally be noted the above description is only a preferred embodiment of the present invention, it is served only for technical solution of the present invention
It is described in more detail.Conceive according to the present invention for those skilled in the art the nonessential improvement of make several and
Adjustment, all belongs to the scope of protection of the present invention.
Claims (5)
1. a kind of method for preparing calcirm-fluoride crystalline ceramics as the vacuum heating-press sintering of auxiliary agent using lithium fluoride, it is characterised in that: tool
Body step includes:
1) preparation of powder raw material: weighing the setting commercially available calcirm-fluoride powder of quality, adds appropriate fluorination lithium powder, anhydrous second is added
Alcohol through ultrasonic disperse, is mixed, is dried for standby；
2) it fills sample: mixed-powder being fitted into graphite jig, and is separated mold and powder with graphite paper；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove and is sintered；
4) processing of ceramics sample: taking out ceramics after sintering, is processed by shot blasting sample to get transparent to calcirm-fluoride
Ceramics.
2. according to claim 1 a kind of calcirm-fluoride crystalline ceramics is prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride
Method, it is characterised in that: calcirm-fluoride used is commercially available with fluorination lithium powder in the step 1), wherein calcirm-fluoride purity >=
99%, lithium fluoride purity >=99.5%.
3. according to claim 1 a kind of calcirm-fluoride crystalline ceramics is prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride
Method, it is characterised in that: in the step 1) calcirm-fluoride and lithium fluoride mixed-powder, the content for adding fluorination lithium powder is
0.2wt%-2.0wt%。
4. according to claim 1 a kind of calcirm-fluoride crystalline ceramics is prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride
Method, it is characterised in that: step 1) the ultrasonic disperse time is 20min-60min.
5. according to claim 1 a kind of calcirm-fluoride crystalline ceramics is prepared by the vacuum heating-press sintering of auxiliary agent of lithium fluoride
Method, it is characterised in that: sintering method is vacuum heating-press sintering in the step 3), and sintering temperature is 700 DEG C -900 DEG C, very
Reciprocal of duty cycle is better than 10Pa, pressure 30MPa-50MPa, soaking time 3h-8h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116375473A (en) * | 2023-03-30 | 2023-07-04 | 山东亚赛陶瓷科技有限公司 | Magnesium fluoride-based composite neutron moderating material and preparation method thereof |
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| US3974249A (en) * | 1970-09-16 | 1976-08-10 | Coors Porcelain Company | Method for manufacturing a transparent ceramic body |
| CN102126857A (en) * | 2011-01-31 | 2011-07-20 | 武汉理工大学 | Method for preparing transparent calcium fluoride ceramic |
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| CN116375473A (en) * | 2023-03-30 | 2023-07-04 | 山东亚赛陶瓷科技有限公司 | Magnesium fluoride-based composite neutron moderating material and preparation method thereof |
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Application publication date: 20190416 |