CN106338449A - Silicon-containing waste composition analysis detection and preservation method - Google Patents
Silicon-containing waste composition analysis detection and preservation method Download PDFInfo
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- CN106338449A CN106338449A CN201610639565.3A CN201610639565A CN106338449A CN 106338449 A CN106338449 A CN 106338449A CN 201610639565 A CN201610639565 A CN 201610639565A CN 106338449 A CN106338449 A CN 106338449A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
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Abstract
The invention belongs to the field of materials, and in particular, relates to a silicon-containing waste composition analysis detection and preservation method particularly including the following steps: 1] preparing an analysis detection agent; 2] detecting the composition of silicon-containing waste by a stepwise elimination method under an isolated oxygen condition; and 3] preserving the silicon-containing waste after the composition is detected under the isolated oxygen condition. The silicon-containing waste composition analysis detection and preservation method provided by the invention can fast and accurately analyze and detect the proportion of a crystal silicon micro-powder and the proportion of a silica micro-powder in the silicon-containing waste respectively during production, and also can avoid the problem that the mutual proportion of the crystal silicon micro-powder and the silica micro-powder is changed in processes of storage and transportation; then most of original abandoned silicon-containing waste becomes a valuable industrial raw material, electric energy and mine resources are greatly saved, carbon dioxide emissions are reduced, and the environmental pollution problem of the silicon-containing waste is effectively solved.
Description
Technical field
The invention belongs to Material Field is and in particular to produce in a kind of cutting in solar wafer and the course of processing contains
The analysis detection of scrap silicon composition and store method.
Background technology
Substantial amounts of cutting waste material can be produced in the cutting process of solar wafer, the main source of these cutting waste materials has
Two parts a: part is the cutting producing when using green silicon carbide cutting blade material cut crystal in solar energy crystalline silicon rod
Waste material, another part is the cutting waste material producing when using diamond cutting secant cut crystal in solar energy crystalline silicon rod,
This two-part main component is: has the used useless green silicon carbide cutting producing in solar wafer cutting process
Sword material fine powder, have the crystal silicon powder being carbonized silicon cutting blade material and cutting down during cut crystal from solar energy crystalline silicon rod,
Fine silica powder (silicon dioxide of the oxidized generation of crystal silicon powder), in addition also water, organic residue material, ferrum and other
Impurity；In addition, also process, in solar wafer, the grinding waste material producing in process of lapping；Both the above waste material all contains
Have substantial amounts of highly purified crystal silicon powder containing scrap silicon.In recent years, with the development of solar energy industry, containing scrap silicon
Yield also increases constantly.But, but it is not fully used containing scrap silicon, and is abandoned, cause a large amount of
Resource and the energy waste, and pollute environment.Containing the useless green silicon carbide cutting blade material fine powder containing in scrap silicon, high-purity
Crystal silicon powder and fine silica powder be that many industries are used for producing raw material needed for product, for example producing carborundum knot
It is required for these raw materials when crystal, silicon carbide ceramics, carborundum are with reference to silicon nitride ceramics, metallic silicon smelting, Antaciron etc.；Special
It is not will to be divided containing the cutting blade material fine powder in scrap silicon, crystal silicon powder and fine silica powder using means such as physics, chemistry
From when becoming separate constituent, the using value containing scrap silicon will get a greater increase.But, siliceous rich in crystal silicon powder
Waste material can progressively be oxidized into fine silica powder in atmosphere, is oxidized into fine silica powder in crystalline silicon micro powder granule
During grain, it is initially to be oxidized to form very thin silica shells on the surface of crystalline silicon micro powder granule, with
The passage of time, silica shells can become increasingly thicker, and the kernel at crystal silicon particle center can become more next
Less, in this change procedure, the mutual ratio of crystal silicon powder and fine silica powder is as the change of time and becomes
Change.And the result of this change will bring great difficulty to recycling siliceous waste material, it is first how aborning
Rapidly, accurately analysis detection is containing the crystal silicon powder in scrap silicon and the ratio shared by fine silica powder；Next to that it is right
Completed to analyze detection containing scrap silicon, how to preserve and just can make the mutual ratio of crystal silicon powder and fine silica powder not
Change again.
Content of the invention
In order to solve to cannot be carried out fast and accurately composition detection and effective technical problem preserving, the present invention containing scrap silicon
A kind of component analyses detection containing scrap silicon and store method are provided.
The technical solution of the present invention is: a kind of component analyses detection containing scrap silicon and store method, its special it
Place is: comprises the following steps:
1] prepare and analyze detection agent:
After precise hydrochloric acid, an auxiliary agent, it is mixed and stirred for uniformly obtaining impurity analysis detection agent with water；
After precise hydrochloric acid, Fluohydric acid. and an auxiliary agent, it is mixed and stirred for uniformly obtaining fine silica powder dividing with water
Analysis detection agent；
After precise nitric acid, Fluohydric acid. and No. two auxiliary agents, it is mixed and stirred for uniformly obtaining the analysis of crystal silicon powder with water
Detection agent；
A described auxiliary agent by one or more inorganic salt, dispersant, activating agent and is constituted, and described No. two auxiliary agents are by one
Plant or plurality of inorganic salt is constituted；Inorganic salt in a number auxiliary agent does not include nitrate；
2] under conditions of starvation adopt substep scalping method detection containing scrap silicon composition:
It is heated to, after moisture evaporating completely, being calculated containing in scrap silicon according to quality difference value containing scrap silicon by be detected
Moisture w；
By to be detected reacted containing scrap silicon and impurity analysis detection agent after, wash and dry to constant weight, according to quality
Mathematic interpolation obtains containing the impurity content v in scrap silicon；
After the analysis detection agent containing scrap silicon and fine silica powder to be detected is reacted, wash and dry to constant weight,
It is calculated containing fine silica powder content t in scrap silicon according to quality difference value；
After the analysis detection agent containing scrap silicon and crystal silicon powder to be detected is reacted, wash and dry to constant weight, root
It is calculated containing the crystalline silicon powder content q in scrap silicon and green silicon carbide fine powder content g according to quality difference value；
3] by preserving under conditions of starvation containing scrap silicon after detection composition.
Step 2] specifically include following steps:
2.1] four parts of siliceous waste material sample to be detected are chosen；
2.2] weigh and obtain first part of siliceous waste material sample quality a, then heating evaporation moisture, to constant weight, weighs again
Obtain quality a, according to quality difference value calculating moisture w:
2.3] weigh and obtain second part of siliceous waste material sample quality b, be subsequently adding impurity analysis detection agent and reacted, instead
Should wash after terminating and dry, weigh again and obtain quality b, according to quality difference value calculating impurity content v:
2.4] weigh and obtain the 3rd part of siliceous waste material sample quality c, be subsequently adding fine silica powder analysis detection agent and enter
Row reaction, reaction is washed after terminating and is dried, and weighs again and obtains quality c, calculates fine silica powder according to quality difference value and contains
Amount t:
2.5] weigh and obtain the 4th part of siliceous waste material sample quality d, be subsequently adding crystal silicon powder analysis detection agent and carry out
Reaction, reaction is washed and is dried after terminating, and weighs again and obtains quality d, according to quality difference value calculate crystalline silicon powder content q and
Green silicon carbide fine powder content g:
Step 2] specifically include following steps:
2.1] choose a siliceous waste material sample to be detected；
2.2] weigh and obtain siliceous waste material sample quality a, then heating evaporation moisture, to constant weight, weighs again and obtains matter
Amount a, according to quality difference value calculating moisture w:
2.3] to step 2.2] quality that obtains be a the siliceous waste material sample of residue in add impurity analysis detection agent to carry out
Reaction, reaction is washed after terminating and is dried, and weighs again and obtains quality b, according to quality difference value calculating impurity content v:
2.4] to step 2.3] quality that obtains be b the siliceous waste material sample of residue in add fine silica powder analysis inspection
Survey agent to be reacted, reaction is washed after terminating and dried, and weighs again and obtains quality c, calculates silicon dioxide according to quality difference value
Powder content t:
2.5] to step 2.4] quality that obtains be c the siliceous waste material sample of residue in add the analysis detection of crystal silicon powder
Agent is reacted, and reaction is washed after terminating and dried, and weighs again and obtains quality d, calculates crystal silicon powder according to quality difference value
Content q and green silicon carbide fine powder content g:
Step 3] be achieved in that: will contain scrap silicon with binding agent mix homogeneously and suppress bonding become pellet or material
Block.
Step 3] be achieved in that: scrap silicon will be contained and be immersed in no in oxygen liquid.
Step 3] be achieved in that: scrap silicon will be contained and be sealed in anaerobic container.
In above-mentioned impurity analysis detection agent, the quality proportioning of each component is:
Water: hydrochloric acid: an auxiliary agent=100ml:5 40ml:0.5 8mg；
The quality proportioning that above-mentioned fine silica powder analyzes each component in detection agent is:
Water: hydrochloric acid: Fluohydric acid.: an auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg；
The quality proportioning that above-mentioned crystal silicon powder analyzes each component in detection agent is:
Water: nitric acid: Fluohydric acid.: No. two auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg.
It is an advantage of the current invention that: the component analyses detection containing scrap silicon provided by the present invention and store method can be real
In now producing, rapidly, accurately analysis detection contains crystal silicon powder and fine silica powder each institute's accounting in scrap silicon
Example, can avoid the mutual ratio of crystal silicon powder and fine silica powder depositing simultaneously, change in transportation
Problem；And then make major part originally become the very valuable raw material of industry by abandoned containing scrap silicon, greatly save
Electric power energy and mine resources, reduce the discharge of carbon dioxide, efficiently solve the problems, such as siliceous waste entrainment environment.
Specific embodiment
The invention provides a kind of can rapidly, accurately analysis aborning detects that the crystalline silicon containing in scrap silicon is micro-
The powder and fine silica powder each technical scheme of proportion and phase that crystal silicon powder and fine silica powder can be made
The preservation scheme that mutually ratio no longer changes；Such scheme not only includes analyzing detection containing agent prescription during scrap silicon
The experimental procedure that species, the ratio of formula, the step of detection and the reagent using different formulations and classification substep are rejected is to containing
Scrap silicon is analyzed detecting, thus obtaining crystal silicon powder, fine silica powder, green silicon carbide fine powder, impurity, moisture respectively
Percentage ratio shared by each composition；Also include cut-off oxygen no longer makes crystal silicon powder continue oxidized guard method simultaneously.
Reagent used in analysis detection for the present invention is impurity analysis detection agent, fine silica powder analysis inspection respectively
Survey agent, crystal silicon powder analysis detection agent；The concrete technical scheme of present pre-ferred embodiments is as follows:
1), prepare impurity analysis detection agent
1.1), chemical reagent
Hydrochloric acid (commercially available chemical reagent)；A number auxiliary agent；
1.2), chemical reagent proportioning
After precise hydrochloric acid, an auxiliary agent, it is mixed and stirred for uniformly obtaining impurity analysis detection agent with water
More preferred, each chemical reagent with the quality proportioning of water is:
Water: hydrochloric acid: an auxiliary agent=100ml:5 40ml:0.5 8mg；
It is more highly preferred to, each chemical reagent with the quality proportioning of water is:
Water: hydrochloric acid: an auxiliary agent=100ml:10 20ml:1 3mg；
2), prepare fine silica powder analysis detection agent
2.1), chemical reagent
Hydrochloric acid (commercially available chemical reagent)；Fluohydric acid. (commercially available chemical reagent)；A number auxiliary agent；
2.2), chemical reagent proportioning
After precise hydrochloric acid, Fluohydric acid. and an auxiliary agent, it is mixed and stirred for uniformly obtaining fine silica powder dividing with water
Analysis detection agent；
More preferred, each chemical reagent with the quality proportioning of water is:
Water: hydrochloric acid: Fluohydric acid.: an auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg；
It is more highly preferred to, each chemical reagent with the quality proportioning of water is:
Water: hydrochloric acid: Fluohydric acid.: an auxiliary agent=100ml:10 20ml:10 20ml:1 3mg；
3), prepare crystal silicon powder analysis detection agent
3.1), chemical reagent
Nitric acid (commercially available chemical reagent)；Fluohydric acid. (commercially available chemical reagent)；No. two auxiliary agents；
3.2), chemical reagent proportioning
After precise nitric acid, Fluohydric acid. and No. two auxiliary agents, it is mixed and stirred for uniformly obtaining the analysis of crystal silicon powder with water
Detection agent；
More preferred, each chemical reagent with the quality proportioning of water is:
Water: nitric acid: Fluohydric acid.: No. two auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg
It is more highly preferred to, each chemical reagent with the quality proportioning of water is:
Water: nitric acid: Fluohydric acid.: No. two auxiliary agent=100ml:10 20ml:10 20ml:1 3mg
The chemical reagent proportioning used in analysis detection agent in the present invention draws after experimental verification repeatedly, when
When hydrochloric acid, nitric acid, Fluohydric acid., the chemical agent concentration such as auxiliary agent, No. two auxiliary agents are too high, the analysis detection agent preparing exists
Easily produce violent chemical reaction in use, not only waste reagent but also be difficult to control to；When the concentration of each chemical agent is too low
When, detection agent chemical reaction is again excessively slow, reduces detection speed and efficiency；Therefore choose suitable chemical reagent proportioning to close
Vital effect is played for Detection results by system；
A number auxiliary agent is to be made up of one or more various inorganic salts (not including nitrate), dispersant, activating agent,
Its Main Function is to produce insoluble matter in prevention reaction product, prevent micropowder reunion from causing to react thorough, protecting in detection
Chemical reaction is stable.Wherein, inorganic salt can select soluble sulphate (such as na2so4、k2so4), phosphate (for example
na3po4、k3po4、na2hpo4、k2hpo4), carbonate (such as na2co3、k2co3), chloride (such as nacl, kcl) etc. common
Salt.Dispersant can be from the inorganic dispersant such as sodium hexameta phosphate, sodium pyrophosphate, sodium tripolyphosphate it is also possible to select three second
The organic dispersing agents such as base hexyl phosphoric acid, polyacrylamide.Activating agent can select enuatrol, sodium stearate, lauryl sulphate acid
The conventional surfactants such as sodium, dodecylbenzene sodium sulfonate.
No. two auxiliary agents are to be made up of one or more various inorganic salts, and its Main Function is to prevent from micropowder from reuniting to cause
During reaction is not thoroughly, protection detects, chemical reaction is stable.Inorganic salt in No. two auxiliary agents can be from various in an auxiliary agent
Salt is it is also possible to select various nitrate (such as nano3、kno3Deng).
4), analyze detecting step:
It is an experimental program that classification substep is rejected, and detecting step has two paths can walk, but final result
It is identical, experimental principle is the same；This two paths is that staged substep is rejected and linear descending substep is rejected respectively；
4.1), staged substep scalping method detecting step:
Choose experiment with to be measured containing scrap silicon, will be divided into close to equal 4 parts containing scrap silicon；
Detection moisture:
Take first part to weigh containing scrap silicon and obtain weight for a, then heating evaporation moisture, to after constant weight, is weighed and obtained weight
For a,
Calculate:
W is containing the percentage ratio shared by moisture in scrap silicon；
Checked for impurities:
Take second part to weigh containing scrap silicon and obtain weight for b, be subsequently adding impurity analysis detection agent, and suitably heat, instead
After should terminating, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight, weighing, to obtain weight be b,
Calculate:
(v+w) it is containing moisture in scrap silicon and the percentage ratio shared by impurity；
(v+w)-w=v
V is containing the percentage ratio shared by impurity in scrap silicon；
Detected silica micropowder:
Take the 3rd part to weigh containing scrap silicon and obtain weight for c, be subsequently adding fine silica powder analysis detection agent, and suitably
Heating, after reaction terminates, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight, weighing, to obtain weight be c,
Calculate:
(t+v+w) it is containing the percentage ratio shared by moisture in scrap silicon and impurity and fine silica powder；
(t+v+w)-(v+w)=t
T is containing the percentage ratio shared by fine silica powder in scrap silicon；
Detection crystal silicon powder:
Take the 4th part to weigh containing scrap silicon and obtain weight for d, be then slowly added into crystal silicon powder analysis detection agent, wait until
After reaction terminates, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight, weighing, to obtain weight be d,
Calculate:
(q+t+v+w) it is containing the percentage ratio shared by moisture, impurity, fine silica powder, crystal silicon powder in scrap silicon；
(q+t+v+w)-(t+v+w)=q
Q is containing the percentage ratio shared by crystal silicon powder in scrap silicon；
Detection green silicon carbide fine powder:
Calculate:
G is containing the percentage ratio shared by green silicon carbide fine powder in scrap silicon；
4.2), linear descending substep scalping method detecting step:
Choose a experiment with to be measured containing scrap silicon；
Detection moisture:
Taking weighs containing scrap silicon obtains weight for a, and then heating evaporation moisture, to after constant weight, is weighed and obtained weight for a,
Calculate:
W is containing the percentage ratio shared by moisture in scrap silicon；
Checked for impurities:
Take the residue that known weight is a to contain scrap silicon, be subsequently adding impurity analysis detection agent, and suitably heat, reaction knot
Shu Hou, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight, weighing, to obtain weight be b,
Calculate:
V is containing the percentage ratio shared by impurity in scrap silicon；
Detected silica micropowder:
Take the residue that known weight is b to contain scrap silicon, be subsequently adding fine silica powder analysis detection agent, and suitably add
Heat, after reaction terminates, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight, weighing, to obtain weight be c,
Calculate:
T is containing the percentage ratio shared by fine silica powder in scrap silicon；
Detection crystal silicon powder:
Take the residue that known weight is c to contain scrap silicon, be then slowly added into crystal silicon powder analysis detection agent, when reaction
After end, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight, weighing, to obtain weight be d,
Calculate:
Q is containing the percentage ratio shared by crystal silicon powder in scrap silicon；
Detection green silicon carbide fine powder:
Calculate:
G is containing the percentage ratio shared by green silicon carbide fine powder in scrap silicon；
Above classification substep is rejected in detecting step, needs not oxygenous gas shield (the such as indifferent gas of overall process
Body, reducibility gas, nitrogen or other protective gas).
5), occluded oxygen gas shielded crystal silicon powder does not continue to oxidized scheme
Protection crystal silicon powder does not continue to oxidized scheme and according to the purposes containing scrap silicon and can contain scrap silicon
In the percentage ratio shared by crystal silicon powder, one of guard method being entered from three kinds of occluded oxygen gas cuts, these three
Guard method is respectively:
5.1), scrap silicon will be contained using binding agent and be bonded to pellet, material block；
When being oxidized to the large percentage of fine silica powder containing the crystal silicon powder in scrap silicon, this containing scrap silicon
It is applied to metal smelting silicon, carborundum etc., this guard method can be adopted；
Cardinal principle is: binding agent is mixed homogeneously with containing scrap silicon and suppresses be bonded to pellet, material block when, containing scrap silicon
The surface of fine powder is wrapped a layer of adhesive, and this layer of binding agent largely protects containing scrap silicon no longer by further oxygen
When changing, and the ball press containing scrap silicon or cuber compacting that are enclosed with binding agent being bonded to pellet, material block, binding agent blocks
Micro gap between fine powder containing scrap silicon, has blocked the intrusion of oxygen, has protected containing scrap silicon well；
5.2) scrap silicon and liquid mixing, will be contained or be immersed in liquid；
When the ratio being oxidized to fine silica powder containing the crystal silicon powder in scrap silicon is less, this containing scrap silicon
It is applied to smelting particulate metal, makes structural ceramicss etc., this guard method can be adopted；
Cardinal principle is: when will contain scrap silicon and liquid mixing or be immersed in liquid, liquid barrier oxygen with siliceous
The possibility of waste material contact, is effectively protected containing scrap silicon；
5.3), will be sealed in the container of no oxygen containing scrap silicon.
When the special hour of ratio being oxidized to fine silica powder containing the crystal silicon powder in scrap silicon, this siliceous useless
Material is applied to making high performance structure ceramic, the purification of crystal silicon powder, can adopt this guard method；
Cardinal principle is: during by being sealed in the container of no oxygen containing scrap silicon, has thoroughly blocked oxygen useless with siliceous
Material contact chance, be effectively protected through component analyses detection after containing scrap silicon；
With reference to specific embodiment, technical scheme and implementation result are described in detail.
1), choose detection with containing scrap silicon
Choose 5 groups of detected samples in a batch is containing scrap silicon, in this 5 groups of detected samples every group have 4 parts right
Compare sample.
In 5 groups of detected samples 4 groups are detected, 1 group is divided using linear descending using the step that staged substep is rejected
The step that step is rejected is detected；
2), using staged substep reject step and argon protection under be analyzed detect:
2.1), detect moisture:
Take first group contain scrap silicon 4 parts of comparative sample, respectively weight is called an, then heating evaporation moisture is to constant weight
Afterwards, respectively weight is called an,
Calculate:
wnIt is the percentage ratio shared by moisture that each part contains in scrap silicon；
Calculate wnBe averagely worth to final result w
First group: (n is 1,2,3,4)
It is 6.02% containing the percentage ratio shared by the moisture in scrap silicon；
2.2), checked for impurities:
Take second group contain scrap silicon 4 parts of comparative sample, respectively weight is called bn, then excessive addition impurity divides respectively
Analysis detection agent, and suitably heats, after reaction terminates, repeatedly washed and filter pressing (suction strainer), heating, drying to constant weight after, respectively
Weight is called bn,
Calculate:
(vn+wn) it is containing moisture in scrap silicon and the percentage ratio shared by impurity；
(vn+wn)-w=vn
vnIt is the percentage ratio shared by impurity that each part contains in scrap silicon respectively；
Calculate vnBe averagely worth to final result v
Second group: (n be 1,2,3,4)
It is 1.05% containing the percentage ratio shared by the impurity in scrap silicon；
2.3), detected silica micropowder:
Take the 3rd group contain scrap silicon 4 parts of comparative sample, respectively weight is called cn, then excessively add titanium dioxide respectively
Silicon powder analyzes detection agent, and suitably heats, and after reaction terminates, is repeatedly washed and filter pressing (suction strainer), heating, drying are to perseverance
Weight after, then respectively weight is called cn,
Calculate:
(vn+wn+tn) it is containing the percentage ratio shared by moisture in scrap silicon and impurity and fine silica powder；
(vn+wn+tn)-(v+w)=tn
tnIt is the percentage ratio shared by fine silica powder that each part contains in scrap silicon respectively；
Calculate tnBe averagely worth to final result t
3rd group: (n be 1,2,3,4)
It is 16.18% containing the percentage ratio shared by the silicon dioxide in scrap silicon；
2.4), detect crystal silicon powder:
Take the 4th group contain scrap silicon 4 parts of comparative sample, respectively weight is called dn, then slowly excessive addition is brilliant respectively
Body silicon powder analyzes detection agent, after reaction terminates, repeatedly washed and filter pressing (suction strainer), after heating, drying to constant weight,
Weigh and obtain weight for dn,
Calculate:
(vn+wn+tn+qn) it is containing the percentage shared by moisture, impurity, fine silica powder, crystal silicon powder in scrap silicon
Than；
(vn+wn+tn+qn)-(v+w+t)=qn
qnIt is the percentage ratio shared by crystal silicon powder that each part contains in scrap silicon respectively；
Calculate qnBe averagely worth to final result q
4th group: (n be 1,2,3,4)
It is 39.02% containing the percentage ratio shared by the crystal silicon powder in scrap silicon；
2.5), detect green silicon carbide fine powder:
The material that residue is got off when detecting the crystal silicon powder of the 4th group of 4 parts of comparative sample containing scrap silicon is exactly carbonization
Silica fine powder, so
Calculate:
gnIt is containing the percentage ratio shared by green silicon carbide fine powder in scrap silicon；
Calculate gnBe averagely worth to final result g
4th group: (n be 1,2,3,4)
It is 37.73% containing the percentage ratio shared by the green silicon carbide fine powder in scrap silicon；
3), using linear descending substep reject step and argon protection under be analyzed detect:
3.1), detect moisture:
Take the 5th group contain scrap silicon 4 parts of comparative sample, respectively weight is called en, then heating evaporation moisture is to constant weight
Afterwards, respectively weight is called en,
Calculate:
wnIt is the percentage ratio shared by moisture that each part contains in scrap silicon；
Calculate wnBe averagely worth to final result w
5th group: (n be 1,2,3,4)
It is 6.04% containing the percentage ratio shared by the moisture in scrap silicon；
3.2), checked for impurities:
Take containing scrap silicon 4 parts of remaining comparative sample it is known that their weight is respectively en, then excessive addition respectively
Impurity analysis detection agent, and suitably heat, after reaction terminates, repeatedly washed and filter pressing (suction strainer), heating, drying are to constant weight
Afterwards, respectively weight is called bn,
Calculate:
vnIt is containing the percentage ratio shared by impurity in scrap silicon；
Calculate vnBe averagely worth to final result v
5th group: (n be 1,2,3,4)
It is 1.06% containing the percentage ratio shared by the impurity in scrap silicon；
3.3), detected silica:
Take containing scrap silicon 4 parts of remaining comparative sample it is known that their weight is respectively bn, then excessive addition respectively
Silicon dioxide analyzes detection agent, and suitably heats, and after reaction terminates, is repeatedly washed and filter pressing (suction strainer), heating, drying are arrived
After constant weight, respectively weight is called cn,
Calculate:
tnIt is the percentage ratio shared by silicon dioxide that each part contains in scrap silicon respectively；
Calculate tnBe averagely worth to final result t
5th group: (n be 1,2,3,4)
It is 16.17% containing the percentage ratio shared by the silicon dioxide in scrap silicon；
3.4), detect crystal silicon powder:
Take containing scrap silicon 4 parts of remaining comparative sample it is known that their weight is respectively cn, then slowly excessive respectively
Add crystal silicon powder analysis detection agent, after reaction terminates, repeatedly washed and filter pressing (suction strainer), heating, drying are to constant weight
Afterwards, respectively weight is called dn,
Calculate:
qnIt is the percentage ratio shared by crystal silicon powder that each part contains in scrap silicon respectively；
Calculate qnBe averagely worth to final result q
5th group: (n be 1,2,3,4)
It is 38.96% containing the percentage ratio shared by the crystal silicon powder in scrap silicon；
3.5), detect green silicon carbide fine powder:
4 parts of remaining comparative sample are carbide fine powder it is known that their weight is respectively dn, so
Calculate:
gnIt is the percentage ratio shared by green silicon carbide fine powder that each part contains in scrap silicon respectively；
Calculate gnBe averagely worth to final result g
5th group: (n be 1,2,3,4)
It is 37.77% containing the percentage ratio shared by the green silicon carbide fine powder in scrap silicon.
Contrasted from above testing result, rejected using staged substep or the detecting step of linear descending substep rejecting enters
Go the result detecting all in the range of requirement of experiment error, therefore, when detecting using any one in two methods all
It is feasible.
Claims (10)
1. a kind of component analyses detection containing scrap silicon and store method it is characterised in that: comprise the following steps:
1] prepare and analyze detection agent:
After precise hydrochloric acid, an auxiliary agent, it is mixed and stirred for uniformly obtaining impurity analysis detection agent with water；
After precise hydrochloric acid, Fluohydric acid. and an auxiliary agent, it is mixed and stirred for uniformly obtaining fine silica powder analysis inspection with water
Survey agent；
After precise nitric acid, Fluohydric acid. and No. two auxiliary agents, it is mixed and stirred for uniformly obtaining the analysis detection of crystal silicon powder with water
Agent；
A described auxiliary agent is made up of one or more inorganic salt, dispersant, activating agent, and described No. two auxiliary agents are by one or more
Inorganic salt is constituted；Inorganic salt in a number auxiliary agent does not include nitrate；
2] under conditions of starvation adopt substep scalping method detection containing scrap silicon composition:
It is heated to, after moisture evaporating completely, being calculated containing the moisture in scrap silicon according to quality difference value containing scrap silicon by be detected
Content w；
By to be detected reacted containing scrap silicon and impurity analysis detection agent after, wash and dry to constant weight, according to quality difference value
It is calculated containing the impurity content v in scrap silicon；
After the analysis detection agent containing scrap silicon and fine silica powder to be detected is reacted, wash and dry to constant weight, according to
Quality difference value is calculated containing fine silica powder content t in scrap silicon；
After the analysis detection agent containing scrap silicon and crystal silicon powder to be detected is reacted, wash and dry to constant weight, according to matter
Amount mathematic interpolation obtains containing the crystalline silicon powder content q in scrap silicon and green silicon carbide fine powder content g；
3] by preserving under conditions of starvation containing scrap silicon after detection composition.
2. the component analyses detection containing scrap silicon according to claim 1 and store method it is characterised in that: step 2] tool
Body comprises the following steps:
2.1] four parts of siliceous waste material sample to be detected are chosen；
2.2] weigh and obtain first part of siliceous waste material sample quality a, then heating evaporation moisture, to constant weight, weighs again and obtains
Quality a, according to quality difference value calculating moisture w:
2.3] weigh and obtain second part of siliceous waste material sample quality b, be subsequently adding impurity analysis detection agent and reacted, reaction knot
Wash after bundle and dry, weigh again and obtain quality b, according to quality difference value calculating impurity content v:
2.4] weigh and obtain the 3rd part of siliceous waste material sample quality c, be subsequently adding fine silica powder analysis detection agent and carry out instead
Should, reaction is washed after terminating and is dried, and weighs again and obtains quality c, according to quality difference value calculating fine silica powder content t:
2.5] weigh and obtain the 4th part of siliceous waste material sample quality d, be subsequently adding crystal silicon powder analysis detection agent and reacted,
Reaction is washed after terminating and is dried, and weighs again and obtains quality d, calculates crystalline silicon powder content q and green carbon according to quality difference value
SiClx fine powder content g:
3. the component analyses detection containing scrap silicon according to claim 1 and store method it is characterised in that: step 2] tool
Body comprises the following steps:
2.1] choose a siliceous waste material sample to be detected；
2.2] weigh and obtain siliceous waste material sample quality a, then heating evaporation moisture, to constant weight, weighs again and obtains quality a,
According to quality difference value calculating moisture w:
2.3] to step 2.2] quality that obtains be a the siliceous waste material sample of residue in add impurity analysis detection agent to carry out instead
Should, reaction is washed after terminating and is dried, and weighs again and obtains quality b, according to quality difference value calculating impurity content v:
2.4] to step 2.3] quality that obtains be b the siliceous waste material sample of residue in add fine silica powder analysis detection agent
Reacted, reaction is washed after terminating and dried, and weighs again and obtains quality c, calculates fine silica powder according to quality difference value
Content t:
2.5] to step 2.4] quality that obtains be c the siliceous waste material sample of residue in add crystal silicon powder analysis detection agent to enter
Row reaction, reaction is washed after terminating and is dried, and weighs again and obtains quality d, calculates crystalline silicon powder content q according to quality difference value
With green silicon carbide fine powder content g:
4. the component analyses detection containing scrap silicon according to claim 1 and store method it is characterised in that: step 3]
Be achieved in that: will contain scrap silicon with binding agent mix homogeneously and suppress bonding become pellet or material block.
5. the component analyses detection containing scrap silicon according to claim 1 and store method it is characterised in that: step 3]
It is achieved in that: scrap silicon will be contained and be immersed in no in oxygen liquid.
6. the component analyses detection containing scrap silicon according to claim 1 and store method it is characterised in that: step 3]
It is achieved in that: scrap silicon will be contained and be sealed in anaerobic container.
7. according to the described component analyses detection containing scrap silicon arbitrary in claim 1-6 and store method it is characterised in that:
In described impurity analysis detection agent, the quality proportioning of each component is:
Water: hydrochloric acid: an auxiliary agent=100ml:5 40ml:0.5 8mg；
The quality proportioning that described fine silica powder analyzes each component in detection agent is:
Water: hydrochloric acid: Fluohydric acid.: an auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg；
The quality proportioning that described crystal silicon powder analyzes each component in detection agent is:
Water: nitric acid: Fluohydric acid.: No. two auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg.
8. the component analyses detection containing scrap silicon according to claim 7 and store method it is characterised in that: described impurity
In analysis detection agent, the quality proportioning of each component is:
Water: hydrochloric acid: an auxiliary agent=100ml:10 20ml:1 3mg.
9. the component analyses detection containing scrap silicon according to claim 7 and store method it is characterised in that: described dioxy
The quality proportioning that each component in detection agent analyzed by SiClx micropowder is:
Water: hydrochloric acid: Fluohydric acid.: an auxiliary agent=100ml:5 40ml:5 40ml:0.5 8mg.
10. the component analyses detection containing scrap silicon according to claim 7 and store method it is characterised in that: described crystalline substance
The quality proportioning that body silicon powder analyzes each component in detection agent is:
Water: nitric acid: Fluohydric acid.: No. two auxiliary agent=100ml:10 20ml:10 20ml:1 3mg.
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| CN117922989A (en) * | 2024-03-21 | 2024-04-26 | 青岛市动物疫病预防控制中心 | Device for taking and storing freeze-dried microsphere reagent for Brucella detection |
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