CN109520777A - Silicon carbide sample spoon and manufacturing process - Google Patents
Silicon carbide sample spoon and manufacturing process Download PDFInfo
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- CN109520777A CN109520777A CN201910018549.6A CN201910018549A CN109520777A CN 109520777 A CN109520777 A CN 109520777A CN 201910018549 A CN201910018549 A CN 201910018549A CN 109520777 A CN109520777 A CN 109520777A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/12—Dippers; Dredgers
- G01N1/125—Dippers; Dredgers adapted for sampling molten metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
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Abstract
The invention discloses a kind of silicon carbide sample spoons, and the sample spoon is with following index: 1300-1380 DEG C of high temperature resistant；Porosity < 0.1%；Density 2.95-3.10 g/cm3.Also disclose a kind of manufacturing process of silicon carbide sample spoon, including molding early period and injection forming step, mid-term machining steps, post-processing steps, slurry used in molding early period and injection forming step includes following component by weight: 75-85 parts of silicon carbide micro-powder, 58-62 parts of softened water, 3.6-4.4 parts of carbon black, 2.7-3.3 parts of carbon fiber, 2.7-3.3 parts of silicon nitride powder, 2.7-3.3 parts of tungsten micro mist, 2.7-3.3 parts of manganese dioxide powder, 2.7-3.3 parts of titanium oxide powder, 3.6-4.4 parts of dispersing agent, 6.5-7.5 parts of binder.
Description
Technical field
The sample spoon for taking molten metal is contained after melting the present invention relates to a kind of metal, and in particular to a kind of metal melting casting
(such as aluminum melting) silicon carbide sample spoon and novel manufacturing process during making, belong to metal casting technique field.
Background technique
Molten metal sample spoon is exclusively used in taking out liquid metals in furnace or in packet, so as to assay.Sample spoon, it is main to wrap
Spoon body and kettleholder are included, kettleholder and spoon body are seamlessly connected.Spoon body is cavity open at one end, corresponding with the opening in the cavity
Another side is connect with kettleholder.It is required that steel pipe bevel is tightly welded with spoon body, steel pipe, which must not be pounded, flat to be welded with spoon body to increase
Add use intensity.
For sample spoon, molten metal sample has the characteristics that high temperature, corrosivity, oxidisability, therefore, takes in selection
When sample spoon, manufacture material will not only have excellent high temperature resistance, also have the property of anticorrosion at high temperature, resistance to oxidation
Can, and to have longer service life, it is easy to that various sizes shape is made according to actual needs.Sample spoon does not have 316 not at present
Become rusty steel, 304 stainless steels, stainless steel lining refractory material, graphite etc..
The selection of sample spoon should be noted that the following:
L, sample spoon material has if appropriate for required melt high temperature, corrosion, oxidation environment；
2, the size and shape being open are easy to take liquid from metal melting vessel and topple over；
3, sample spoon should have more smooth inside and outside wall, and melt is prevented to be sticked on sample spoon；
4, sample spoon mouth should be made perpendicular to melt, thick lateral constant speed interception complete to flow of slurry overall with when sampling；
It 5, need to be by certain, equal time interval when sampling；
6, sample spoon will be inspected periodically, and the oxidation of sample spoon material or destruction, cause slag caused by preventing because of melt high temperature or corrosion
Pollute sample liquid；
7, each sample point should configure dedicated sample spoon；
8, volume needed for sample spoon volume should be greater than the melt once intercepted.
Due to the functional requirement of sample spoon, its material and use environment are complicated at present, contour structures type is more, accuracy
It is more demanding, surface smoothness requirements are stringent, entire product members wall unevenness is even.It is molten vulnerable to metal such as stainless steel sample spoon
Liquid oxidation corrosion, service life is short, and replacement frequency is fast；Stainless steel lining refractory material sample spoon is toasted vulnerable to high-temperature metal melt,
Its wadding easily peels off, and sampling accuracy is poor, influences service life, and be easy scaling-off pollution melt.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the above-mentioned deficiency of the prior art, provide in a kind of metal smelting process
With silicon carbide sample spoon, with solve existing material is perishable, oxidizable, the porosity is high, poor accuracy, easy slag contaminated samples,
It cannot achieve the technological deficiencies such as the production of special-shaped sample spoon.
To solve the above problems, the invention adopts the following technical scheme: silicon carbide sample spoon, the sample spoon have following finger
Mark:
1300-1380 DEG C of high temperature resistant；
Porosity < 0.1%；
Density 2.95-3.10 g/cm3。
The present invention selects silicon carbide material to manufacture sample spoon, not only can have its excellent high temperature resistance, and can be with
Corrosion-resistant and resistance to oxidation, even if can be widely applied in metal smelt industry in the strong metallic solution of high temperature and corrosivity, being
It realizes metal sampler, accurately measure required important component, for its weight, silicon carbide sample spoon density is 2.95g/
cm3 - 3.2g /cm3, with sized products can 2 times or more more light than stainless steel, use is lighter；Long service life, carbonization
The silicon ceramics porosity is less than 0.1%, and the common refractory porosity is that 18%-30% is differed, and more resistance to oxidation is corrosion-resistant.
The present invention also provides the manufacturing process of above-mentioned silicon carbide sample spoon, including molding early period and injection forming step,
Mid-term machining steps, post-processing steps, slurry used in molding early period and injection forming step wrap by weight
Include following component:
75-85 parts of silicon carbide micro-powder, 58-62 parts of softened water, 3.6-4.4 parts of carbon black, 2.7-3.3 parts of carbon fiber, silicon nitride powder
2.7-3.3 parts, 2.7-3.3 parts of tungsten micro mist, 2.7-3.3 parts of manganese dioxide powder, 2.7-3.3 parts of titanium oxide powder, dispersing agent
3.6-4.4 6.5-7.5 parts of part, binder.
Be below the present invention above scheme is advanced optimized: the mid-term machining steps the following steps are included: 1.,
After the hair body drying of spoon body, surfacing is carried out；2., with machine tooling kettleholder.
Advanced optimize: 2. the step is using machine tooling kettleholder shape to the margin of tolerance ± 1mm.
Advanced optimize: 2. the step is to use machine tooling kettleholder shape to surface roughness for Ra1.6-3.2.
Advanced optimize: the post-processing steps are the following steps are included: a, molding blank first dry Indoor Dry in high temperature
Dry, then shove charge is sintered；B, blasting treatment.
Advanced optimize: in the step a, it is 82-97 DEG C that high temperature, which dries room temperature,.
Advanced optimize: in the step a, molding blank is 8-10 hours in high temperature drying indoor drying time.
Advanced optimize: in step a, molding blank is dried to moisture content to be lower than after 2% in high temperature drying room and be carried out
Sintering.
Advanced optimize: the blasting treatment makes product surface roughness Ra0.2-1.6.
The present invention can accurately complete the manufacture of the inside and outside structure type of sample spoon, can produce special-shaped, asymmetric, uneven
Even sample spoon；And Product Process is simple, high yield rate.
It is the comparison of the present invention with the prior art below:
Present invention will be further explained below with reference to the attached drawings and examples.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of sample spoon in embodiment of the invention；
Fig. 2 is the top view of Fig. 1；
Fig. 3 is the structural schematic diagram of sample spoon in embodiment of the invention；
Fig. 4 is the top view of Fig. 3；
Fig. 5 is the structural schematic diagram of sample spoon in embodiment of the invention；
Fig. 6 is the top view of Fig. 5.
Specific embodiment
Embodiment 1, as shown in figures 1 to 6, silicon carbide sample spoon, including the metallic solution sampling using silicon carbide material production
Spoon, can make that corrosion-resistant sample spoon, resistance to oxidation, the porosity are low, accuracy is high, are not easy contaminated samples in this way.
The present invention selects silicon carbide material to manufacture sample spoon, not only can have its excellent high temperature resistance, and can be with
Corrosion-resistant and resistance to oxidation, even if can be widely applied in metal smelt industry in the strong metallic solution of high temperature and corrosivity, being
It realizes metal sampler, accurately measure required important component, for its weight, silicon carbide sample spoon density is 2.95g/
cm3 -3.1g/cm3, with sized products can 2 times or more more light than stainless steel, use is lighter；Long service life, silicon carbide
The ceramic porosity is less than 0.1%, and the common refractory porosity is that 18%-30% is differed, and more resistance to oxidation is corrosion-resistant.
The present invention also provides a kind of manufacturing process of above-mentioned silicon carbide sample spoon, comprising the following steps:
(1) bed die and outer bed die in making: with the structure ruler of the inside and outside bed die designed according to the structure of sample spoon spoon body and kettleholder
Very little is foundation, using machining, artisan craftsmanship adhering method, completes the production of spoon body and the inside and outside bed die of kettleholder, outer bottom mold materials
Select one of aluminium alloy, gypsum, epoxy resin, one of the interior bed die material selection aluminium alloy, gypsum.
(2) make production external mold with outer bottom molding: production external mold is first uniformly smeared outer bed die appropriate soft using plaster mold
Outer bed die is placed in plaster mold shape mold and is fixed by soap water, and stone is made according to the proportions of land plaster and water 3:2
Cream slurry, gypsum and water be stirred under vacuum 1-3 minutes after being sufficiently mixed, and screen out impurity after mixing evenly, calcium plaster is injected mould
In type, slight oscillatory excludes bubble, and calcium plaster is made to flow into each tiny edges and corners, it is ensured that calcium plaster disposably fills mold
Die cavity removes outer bed die after calcium plaster solidification, takes out production external mold, it is 40-50 DEG C in temperature after being molded as that gypsum, which produces outer,
Between hothouse in drying 3-4 days, using electronic scale weighing, calculate when mold moisture content is lower than 10% out of hothouse
It takes out, and further quantity has Measurement die size, mold tolerance is less than in the case of 1mm, can come into operation.
(3) coring processed: production internal model is manufactured with interior bed die, then by molded shape core in producing；
The production internal model of interior bed die the manufacture spoon body and kettleholder of spoon body and kettleholder is respectively adopted, then uses the production of spoon body and kettleholder
Internal model manufactures the type core of spoon body and kettleholder respectively；According to the internal structure of spoon body and kettleholder, the inside of manufacture and spoon body and kettleholder
The type core that structure matches.
(4) it sizes mixing and injection forming: before booting, checking whether clutch, brake of ingredient blender etc. be good, stirs
It mixes centainly clean out in machine barrel and has foreign matter, check that the insulation of electrical equipment and ground connection remain intact；
Booting carries out noload test run in use, should first start blender, adds raw material stirring production again after machinery works well
Slurry, the slurry include following component by weight: 60 parts of softened water, 80 parts of silicon carbide micro-powder, 4 parts of carbon black, 3 parts of carbon fiber,
3 parts of silicon nitride powder, 3 parts of tungsten micro mist, 3 parts of manganese dioxide powder, 3 parts of titanium oxide powder, 4 parts of dispersing agent, 7 parts of binder；
Wherein: the softened water in raw material largely volatilizees in demoulding and drying, dispersing agent and binder sinter to 1000 ±
It volatilizees thoroughly at 10 DEG C or so, metallic silicon, which is penetrated into pyroreaction in green body, reacts and fill up all stomatas.
The raw material needs the high-speed stirred in the case where revolving speed is the operating condition of 850-900r/min in blender is added, when stirring
Between need 32 hours or more, so that all raw materials is sufficiently mixed obtained slurry, after slurry configures, by slurry contain take out, filter it is standby
With；
By dried mold, it is placed into slip casting area, using solid casting method, filtered slurry is injected in mold, slip casting
When operation, it is necessary to position, the quantity and size for determining injected hole on production mould according to spoon body and the structure of kettleholder, then by type
Core is fixed in production external mold, has to that the two center line is kept to be overlapped, then mold slip casting；Note is rationally grasped during slip casting
Speed is starched, injection speed is about 25-40s/L, it is ensured that slurries will not generate bubble, swash phenomena such as splashing when injecting, and shake frequently
Dynamic production mould, keeps pulp flow uniform.
(5) dry: the mold after slip casting being stood 40-50 hours, mold is opened, silicon carbide green body is taken out, after demoulding
The molded blank of spoon body and kettleholder is obtained, it, can be by green body if outdoor temperature is at 15 DEG C or more, and when air humidity is less than 70%RH
Spontaneously dry 5-8 hours in outdoor, type core and green body (blank) are detached from again after dry, then claim blank electronic scale
Restatement calculates estimated moisture content, is then fed into electric baking booth low temperature drying, and temperature is arranged in 25-29 in electric baking booth
It is 40-60 hours dry between DEG C, then blank electronic scale is weighed, moisture content is calculated, is taken when moisture content is less than 5%
Out.
(6) biscuit machining, finishing
It is broadly divided into two steps:
The first step, after the hair body drying of spoon body, by manually being modified to the defect in billet surface；
Second step sets vertical or horizontal machine tool lathe tool row according to the length of kettleholder to be processed, diameter equidimension parameter
Blank after drying is clamped on the chuck of lathe by journey, and is corrected by measurer to blank, and then Cutting tool installation manner exists
On knife rest and to knife, then required according to the size of kettleholder shape, with slide calliper rule and bevel protractor (measurer) further amendment lathe tool with
After the angle of blank axis, start lathe, kettleholder shape is processed by lathe tool, constantly uses gage measuring spoon in process
Handle length, diameter equidimension, the guarantee kettleholder blank shape margin of tolerance use surface roughness comparative sample within ± 1mm
Block (abbreviation sample block) is according to vision and tactile compared with blank measured surface, it is ensured that surface roughness between Ra1.6-3.2 and
Sight check blank surface is without dark line, breakage, stomata etc.；
Biscuit integrally passes through after the completion of machining, kettleholder and spoon body is spliced, then to the defective shaping and drying base in surface
It is modified.
(7) it is sintered: the molding blank trimmed is sent into high temperature drying room, it is 8-10 hours dry between 82-97 DEG C, lead to
Green body weight change is crossed, green body moisture content is calculated and is less than 2%, can be fitted into vacuum sintering furnace after the completion, by metallic silicon
Product gap and bottom are poured into, metallic silicon (99.5% or more the silicon metal purity) weight being scattered is about product blank weight
1 times of amount, weight differential floats up and down no more than 25%.
Before vacuum sintering furnace sintering booting, cooling water is first connected, water pressure of cooling water should be kept between 0.1~0.2 Mpa, out
Each water valve flow on vacuum sintering furnace is transferred to suitable position, the then pressurising into vacuum sintering furnace by coolant-temperature gage≤45 DEG C
Contracting air makes vacuum-sintering furnace pressure reach 0.3-0.5MPa, then passes through the temperature controller on vacuum sintering furnace
(FP23) heating process curve is set, then vacuum sintering furnace inhales vacuum, drops to vacuum degree in furnace between 10-50pa；
Then it is heated, and runs FP23 heating schedule, heated in the backward vacuum sintering furnace of beginning and pour industrial nitrogen
(99.6% or more purity) opens the exhaust blower and Wei Chong on vacuum sintering furnace when being inflated to the setting upper limit (1 ± 0.05Kpa)
Valve, adjusting micro- air inflow for rushing valve upper rotor part flowmeter is 400 ± 5L/h, issues report when temperature is increased to 800 DEG C of alarm devices
It is alert, at the same it is micro- rush valve and exhaust valve is automatically closed, release alarm in alert interface and close exhaust blower in monitoring interface, and continue
1700 ± 5 DEG C are warming up to, while being evacuated down between 50-200pa, operator is observed at any time by the observation window on furnace body
The temperature variations that infrared radiation thermometer is shown in hot-zone；
Wherein, when vacuum-sintering in-furnace temperature rises to 1410 DEG C, metallic silicon starts to melt, as temperature continues to increase, metal
Silicon continues to melt and generate steam, adsorbs and penetrates into silicon carbide blank body, and the carbon in green body is reacted with the Si of infiltration, generates β-
SiC, and with α-SiC(silicon carbide micro-powder) combine, free Si is filled with stomata, becomes the ceramic material of high compactness；
When temperature is to 1700 ± 5 DEG C, heating schedule end of run, vacuum drying oven (vacuum sintering furnace) heating system, which is automatically closed, stops
Only, after constant temperature waits 0.5-1.5 hours, inflated with nitrogen (99.6% or more purity) is to 1 ± 0.05Kpa and cooling, when temperature is lower than
After 600-700 DEG C, the air cooling system on openable vacuum sintering furnace assists cooling, reaches tapping temperature (about 150 DEG C or less)
Afterwards, air cooling system is closed, prepares to come out of the stove.
(8) blasting treatment: after the product sintered of coming out of the stove is down to room temperature (about 10-45 DEG C), it is separated from silica sand and is taken
Out, then by product it is placed in sand-blasting machine, diamond dust movement, diamond dust and production is blown by the gas that air compressor machine in sand-blasting machine generates
Product surface contact friction is removed the silicon metal of product surface adhesion, keeps product surface round and smooth bright and clean, compared using surface roughness
Sample block (abbreviation sample block) is according to vision and tactile compared with product measured surface, it is ensured that product surface roughness is in Ra0.2-1.6
Between；That is product surface takes out later, stores without adhesion metallic silicon and other visual foreign matters, packs after to be cleaned.
Above-mentioned steps (1)-(5) are molding early period and injection forming step, and step (6) is mid-term machining steps, step
(7), (8) are post-processing steps.
Embodiment 2, embodiment 1 the step of in (4), the slurry includes following component by weight: 58 parts of softened water,
75 parts of silicon carbide micro-powder, 3.6 parts of carbon black, 2.7 parts of carbon fiber, 2.7 parts of silicon nitride powder, 2.7 parts of tungsten micro mist, manganese dioxide
2.7 parts of powder, 2.7 parts of titanium oxide powder, 3.6 parts of dispersing agent, 6.5 parts of binder；And using technique production documented in embodiment 1
Silicon carbide sample spoon.
Embodiment 3, embodiment 1 the step of in (4), the slurry includes following component by weight: 62 parts of softened water,
85 parts of silicon carbide micro-powder, 4.4 parts of carbon black, 3.3 parts of carbon fiber, 3.3 parts of silicon nitride powder, 3.3 parts of tungsten micro mist, manganese dioxide
3.3 parts of powder, 3.3 parts of titanium oxide powder, 4.4 parts of dispersing agent, 7.5 parts of binder；And using technique production documented in embodiment 1
Silicon carbide sample spoon.
The present invention can accurately complete the manufacture of the inside and outside structure type of sample spoon, can produce special-shaped, asymmetric, uneven
Even sample spoon；And Product Process is simple, high yield rate.
It is the comparison of the present invention with the prior art below:
| Material | 304/316 stainless steel | Silicon carbide |
| Density g/cm3 | 7.70-8.00 | 2.95-3.10 |
| Production method | Rolling | Slip casting |
| Product structure | Simply | It is complicated |
| Corrosion resistance | Generally | It is excellent |
| Oxidation resistent susceptibility | Generally | It is excellent |
| High temperature resistance | 304 stainless steels using temperature at 800 DEG C hereinafter, the use temperature of 316 stainless steels is at 1000 DEG C or less | Using temperature up to 1380 DEG C |
| Service life | Less than 30 days | 60 days or more |
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for those skilled in the art
For member, it is clear that invention is not limited to the details of the above exemplary embodiments, and without departing substantially from spirit of the invention or substantially
In the case where feature, the present invention can be realized in other specific forms, therefore, in all respects, should all will implement
Example regards exemplary as, and is non-limiting, and the scope of the present invention is by appended claims rather than above description limits
It is fixed, it is intended that including all changes that fall within the meaning and scope of the equivalent elements of the claims in the present invention.
Claims (10)
1. silicon carbide sample spoon, it is characterised in that: the sample spoon has following index:
1300-1380 DEG C of high temperature resistant；
Porosity < 0.1%；
Density 2.95-3.10 g/cm3。
2. the manufacturing process of silicon carbide sample spoon as described in claim 1, it is characterised in that: the technique include molding early period and
Injection forming step, mid-term machining steps, post-processing steps are starched used in molding early period and injection forming step
Material includes following component by weight:
75-85 parts of silicon carbide micro-powder, 58-62 parts of softened water, 3.6-4.4 parts of carbon black, 2.7-3.3 parts of carbon fiber, silicon nitride powder
2.7-3.3 parts, 2.7-3.3 parts of tungsten micro mist, 2.7-3.3 parts of manganese dioxide powder, 2.7-3.3 parts of titanium oxide powder, dispersing agent
3.6-4.4 6.5-7.5 parts of part, binder.
3. the manufacturing process of silicon carbide fastener according to claim 2, it is characterised in that: the mid-term machining steps
The following steps are included: 1., after the hair body drying of spoon body, carry out surfacing；2., with machine tooling kettleholder.
4. the manufacturing process of silicon carbide sample spoon according to claim 3, it is characterised in that: 2. the step is using machine
Bed processes kettleholder shape to the margin of tolerance ± 1mm.
5. the manufacturing process of silicon carbide sample spoon according to claim 3, it is characterised in that: 2. the step is using machine
Bed processing kettleholder shape to surface roughness is Ra1.6-3.2.
6. the manufacturing process of silicon carbide fastener according to claim 2, it is characterised in that: the post-processing steps packet
Include following steps: a, molding blank first dry indoor seasoning in high temperature, and then shove charge is sintered；B, blasting treatment.
7. the manufacturing process of silicon carbide sample spoon according to claim 6, it is characterised in that: in the step a, high temperature dries
Dry room temperature is 82-97 DEG C.
8. the manufacturing process of silicon carbide sample spoon according to claim 7, it is characterised in that: in the step a, at parison
Body is 8-10 hours in high temperature drying indoor drying time.
9. the manufacturing process of silicon carbide sample spoon according to claim 8, it is characterised in that: in step a, molding blank
It is dried in high temperature drying room to moisture content to be lower than after 2% and be sintered.
10. the manufacturing process of silicon carbide sample spoon according to claim 6, it is characterised in that: the blasting treatment makes to produce
Product surface roughness is Ra0.2-1.6.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115894038A (en) * | 2022-12-30 | 2023-04-04 | 山东中鹏特种陶瓷有限公司 | Manufacturing process of large-size silicon carbide sand mill lining |
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