CN102041138B - Additive for improving utilization ratio of silicon crystal line cutting mortar as well as preparation method and application method of addictive - Google Patents
Additive for improving utilization ratio of silicon crystal line cutting mortar as well as preparation method and application method of addictive Download PDFInfo
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Abstract
The invention discloses an additive for improving utilization ratio of silicon crystal line cutting mortar as well as a preparation method and application method of the addictive. The additive is composed of the following raw materials in percentage by weight: 50-96.5% of polyethylene glycol, 1-10% of penetrating agent, 1-20% of ether alcohol surfactant, 0.5-10% of extreme pressure resistant chelator and 1-10% of assistant detergent. The preparation method comprises the steps of weighing and mixing the raw materials. The application process comprises the following steps: 1. carrying out the first line cutting the mortar and recovering the mortar; 2. adding the additive: adding the additive to the recovered mortar after the first linear cutting based on the weight ratio of 1:100 plus/minus 10, and then evenly stirring; 3. carrying out the second line cutting; and 4. carrying out the third line cutting and recovering the mortar. The addictive is reasonable in design and has good use effect and practicable value, addictive preparation and use processes are simple, operation is convenient, and the defects of the existing silicon wafer cutting fluid such as more severe pollution, higher rejection rate, high production cost, low utilization ratio and the like can be overcome.
Description
Technical field
The invention belongs to silicon wafer line cutting technology field, especially relate to a kind of additive and preparation and using method that improves silicon wafer linear cutting mortar utilization ratio.
Background technology
Silicon chip is the base mateiral of industries such as semi-conductor, sun power and liquid-crystal display, be divided into monocrystalline silicon piece and polysilicon chip, its raw material is monomer silicon single crystal or polysilicon, pulls into silicon ingot through ingot furnace, be cut into silicon rod again, use wire cutting machine to be processed into the silicon chip of all size afterwards.
Polyethylene glycol type silicon wafer wire cutting liquid is to be the composite product that mixes with components such as antioxidant, sequestrant and tensio-active agents of principal constituent with the polyoxyethylene glycol, is leading in the market silicon wafer cutting liquid.This series products has nontoxic, nonirritant, and good water-solubility is arranged, and with many organic matter components good characteristics such as intermiscibility is arranged.Cutting use properties side, this product with its uphang buoyancy, high lubricity and high dispersive characteristic with cutting such as silicon carbide abrasive material equably attached on the cutting wire, thereby and move fast by steel wire and to drive abrasive material and realize dicing processing polysilicon (silicon single crystal).The silicon wafer wire cutting liquid is a requisite important supplement production material in the photovoltaic industry.
The silica flour that produces when containing the cutting silicon rod through the mortar after the cutting, broken small silicon-carbide particle and micro-iron powder and the partial oxidation iron of steel wire through producing after the grinding, moisture and metal ion content also obviously increase simultaneously.Solid particulate that rolls up and moisture have reduced the viscosity of mortar, influence the biofilm band slurry ability of its suspension stability and steel wire, and the mortar cutting ability is reduced.The reunion of molecule very easily causes the cut of silicon chip surface, and simultaneously, under the effect of newly-increased surface energy, silicon face adsorbs various impurity, and very easily forms chemisorption, produces various uneven surfaces spots and is difficult to clean.Particularly with in iron micro mist and partial oxidation iron and the liquid based on the metal ion of iron ion in working angles, because approach exhaustions such as antioxidant, sequestrant and tensio-active agent, can and infiltrate wafer inside attached to wafer surface, cause metallic pollution, these have all had a strong impact on the quality of silicon chip, and production is caused very big loss.
At present, silicon chip cutting enterprise has to use new mortar or replenishes fresh cutting liquid with the recovery waste mortar reduce production costs for guaranteeing the silicon chip quality in process of production.Produce actual showing, cut useless sheet (cut, piebald etc.) that silicon rod produces first less than 1% with fresh mortar, once cutting finishes and accounts for 3% of total amount by the useless sheet that carries out cutting silicon rod and being produced the second time with this mortar after the ON-LINE SEPARATION, the useless sheet that cuts silicon ingot for the third time and produced accounts for 7% of total amount, has not had using value.So, generally on producing, can improve the utilization ratio of cutting mortar to reduce production costs with online recovery mortar.But, because the consumption of important component such as original antioxidant, sequestrant and tensio-active agent makes the performance serious degradation of mortar in the mortar use, as band sand ability weaken, metal ion content increases and oxidation chromogenesis etc.These factors have had a strong impact on the cutting and the cleaning of silicon chip, produce a large amount of useless sheets, have improved production cost.So mortar can only utilize twice and can not be used for cutting for the third time aborning.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, provide a kind of input cost low, add the additive of convenient and the raising silicon wafer linear cutting mortar utilization ratio that result of use is good, practical value is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of additive that improves silicon wafer linear cutting mortar utilization ratio, it is characterized in that: by 50%～96.5% polyoxyethylene glycol by weight percentage, 1%～10% permeate agent, 1%～20% ether alcohol class tensio-active agent, 0.5%～10% anti-extreme pressure sequestrant and 1%～10% washing assistant uniform mixing form, the molecular weight of described polyoxyethylene glycol is 200D～600D, described permeate agent is the fatty alcohol-polyoxyethylene ether with 5～10 carbon atoms, described anti-extreme pressure sequestrant is fatty alcohol sulfate monoethanolamine salt ASEA or alcohol ether phosphate monoester ethanolamine salt, and described washing assistant is one or both among polyvinylpyrrolidone PVP-k25 and the polyvinylpyrrolidone PVP-k30.
The additive of above-mentioned raising silicon wafer linear cutting mortar utilization ratio is characterized in that: described ether alcohol class tensio-active agent is fatty alcohol polyoxyethylene ether sulfate AES.
The additive of above-mentioned raising silicon wafer linear cutting mortar utilization ratio is characterized in that: described ether alcohol class tensio-active agent is one or both in AEO-7 nonionogenic tenside and the AEO-12 nonionogenic tenside.
Simultaneously, it is simple and realize improving easily the preparation method of the additive of silicon wafer linear cutting mortar utilization ratio to the invention also discloses a kind of preparation method's step, it is characterized in that this method may further comprise the steps:
Step 1, each component weighing: according to weight percent is 50%～96.5%: 1%～10%: 1%～20%: 0.5%～10%: 1%～10% ratio, polyoxyethylene glycol, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant are carried out weighing respectively;
Step 2, mixed preparing: under 35 ℃～120 ℃ temperature condition, after the polyoxyethylene glycol of institute's weighing in the step 1, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant mixed and fully stirring 5 minutes～10 minutes, make additive.
The preparation method of the additive of above-mentioned raising silicon wafer linear cutting mortar utilization ratio, it is characterized in that: described in the step 2 under 35 ℃～120 ℃ temperature condition, during with the polyoxyethylene glycol of institute's weighing in the step 1, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant uniform mixing, after by heating installation polyoxyethylene glycol being heated to 35 ℃～120 ℃ earlier, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant being added in the polyoxyethylene glycol mix again.
In addition, the present invention also provides a kind of using method that step is simple, addition is controlled the additive of convenient and the raising silicon wafer linear cutting mortar utilization ratio that result of use is good of adding, and it is characterized in that this method may further comprise the steps:
Step I, line cutting for the first time and mortar reclaim: adopt the wire cutting liquid for preparing in advance that silicon single crystal or polysilicon are carried out the line cutting first time, and in the line cutting process linear cutting mortar is reclaimed, the linear cutting mortar that is reclaimed this moment is the mortar after line cuts for the first time; Described wire cutting liquid for conventional uses cut liquid with polyoxyethylene glycol as the silicon single crystal cutting liquid or the polysilicon of principal constituent;
Step II, additive are added: the additive that mixed preparing is good joins in the mortar after the line cutting first time of reclaiming among the step I with 1: 100 ± 10 weight ratio under the continuously stirring state, and stir, make the linear cutting mortar that is added with additive;
Step II I, line cutting for the second time: adopt the linear cutting mortar that is added with additive described in the Step II that silicon single crystal or polysilicon are carried out the line cutting second time;
Step IV, line cutting for the third time: adopt the mortar after line cuts for the second time among the Step II I that silicon single crystal or polysilicon are carried out line cutting for the third time;
The cutting process of line for the third time described in the line cutting second time described in the line cutting first time described in the step I, the Step II I and the step IV, all adopt multi-line cutting machine and routinely wire cutting technology cut.
The using method of the additive of above-mentioned raising silicon wafer linear cutting mortar utilization ratio is characterized in that: when fully stirring in the Step II, churning time is 60 minutes～120 minutes.
The using method of the additive of above-mentioned raising silicon wafer linear cutting mortar utilization ratio, it is characterized in that: when the additive that mixed preparing is good joined in the mortar after the line cutting first time of reclaiming among the step I under the continuously stirring state in the Step II, described additive was 1: 100 with the weight ratio of the back of line cutting for the first time mortar.
The present invention compared with prior art has the following advantages:
1, improved the utilization ratio of silicon wafer linear cutting mortar effectively, can significantly reduce production costs.During actual the use, in the mortar that cutting is for the first time reclaimed, add additive of the present invention, carry out second time and line cutting for the third time again, and cut doping more before for the third time, thereby only need add an additive and get final product.
2, prepared additive has good infiltration, lubricated and sequestering action, has obviously reduced surface damage, mechanical stress and the thermal stresses of section, has increased the silicon chip yield rate.
3, solve the silicon wafer linear cutting mortar effectively and used later stage smear metal and the sedimentary again problem of pelletizing powder, avoided the chemical bonding-adsorption of silicon chip surface, be convenient to the cleaning and the following process of silicon chip.
4, select the highly effective chelating agent for use, effectively controlled the pollution of metal ion, help improving the quality of products silicon chip.
5, additive preparation and use are easy, only need during preparation each component is all got final product with mixing according to the design proportioning, and in the mortar after the line first time that when using above-mentioned additive is joined online recovery under constantly stirring cuts and behind the stirring and evenly mixing, the cutting second time can be carried out, additive needn't be added again when cutting for the third time.
6, practical value height, by adding minor amounts of additives in the linear cutting mortar after using for the first time, can obviously improve the over-all properties of mortar, improve the utilization ratio of semi-conductor silicon wafer linear cutting mortar effectively, can make the mortar recycling to three cuttings and four cuttings, and useless sheet rate meets the demands, thereby can significantly reduce the production cost of silicon wafer.In the actual mechanical process, additive of the present invention is added in the mortar that reclaim the cutting back for the first time, the useless sheet rate that can make back cutting twice silicon rod produce has reduction effect preferably.
7, applied widely, can effectively be suitable for to the line cutting of silicon single crystal, polysilicon and other compound semiconductor, and can significantly improve the utilization ratio of above-mentioned linear cutting mortar.
In sum, the present invention is reasonable in design, additive preparation and use simple, it is convenient to control and result of use, practical value height, can effectively solve number of drawbacks and deficiencies such as serious, the useless sheet rate of pollution that existing silicon chip cutting fluid exists is higher, production cost is high, utilization ratio is low.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Method flow block diagram when Fig. 1 uses additive for the present invention.
Embodiment
The additive of raising silicon wafer linear cutting mortar utilization ratio of the present invention, by 50%～96.5% polyoxyethylene glycol by weight percentage, 1%～10% permeate agent, 1%～20% ether alcohol class tensio-active agent, 0.5%～10% anti-extreme pressure sequestrant and 1%～10% washing assistant uniform mixing form, the molecular weight of described polyoxyethylene glycol is 200D～600D, described permeate agent is the fatty alcohol-polyoxyethylene ether with 5～10 carbon atoms, described anti-extreme pressure sequestrant is fatty alcohol sulfate monoethanolamine salt ASEA or alcohol ether phosphate monoester ethanolamine salt, and described washing assistant is one or both among polyvinylpyrrolidone PVP-k25 and the polyvinylpyrrolidone PVP-k30.In the actual fabrication process, can adjust accordingly above-mentioned each components contents according to the concrete needs of reality.
When the additive that improves silicon wafer linear cutting mortar utilization ratio was prepared, its preparation method may further comprise the steps:
Step 1, each component weighing: according to weight percent is 50%～96.5%: 1%～10%: 1%～20%: 0.5%～10%: 1%～10% ratio, polyoxyethylene glycol, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant are carried out weighing respectively.
Step 2, mixed preparing: under 35 ℃～120 ℃ temperature condition, after the polyoxyethylene glycol of institute's weighing in the step 1, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant mixed and fully stirring 5 minutes～10 minutes, make additive.
In the actual mechanical process, under 35 ℃～120 ℃ temperature condition, during with the polyoxyethylene glycol of institute's weighing in the step 1, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant uniform mixing, after by heating installation polyoxyethylene glycol being heated to 35 ℃～120 ℃ earlier, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant being added in the polyoxyethylene glycol mix again.During actual fabrication, can adjust the temperature condition and the churning time of mixed preparing, and each component thorough mixing is even, stir continuously after thorough mixing stirs and under the continuously stirring state, add in the linear cutting mortar according to the concrete needs of reality.
A kind of method that the additive that improves silicon wafer linear cutting mortar utilization ratio is used as shown in Figure 1 may further comprise the steps:
Step I, line cutting for the first time and mortar reclaim: adopt the wire cutting liquid for preparing in advance that silicon single crystal or polysilicon are carried out the line cutting first time, and in the line cutting process linear cutting mortar is reclaimed, the linear cutting mortar that is reclaimed this moment is the mortar after line cuts for the first time; Described wire cutting liquid for conventional uses cut liquid with polyoxyethylene glycol as the silicon single crystal cutting liquid or the polysilicon of principal constituent.
Step II, additive are added: the additive that mixed preparing is good joins in the mortar after the line cutting first time of reclaiming among the step I with 1: 100 ± 10 weight ratio under the continuously stirring state, and stir, make the linear cutting mortar that is added with additive.That is to say that the weight ratio between the mortar after described additive and the line cutting for the first time is 1: 100 ± 10.
Step II I, line cutting for the second time: adopt the linear cutting mortar that is added with additive described in the Step II that silicon single crystal or polysilicon are carried out the line cutting second time.
Step IV, line cutting for the third time: adopt the mortar after line cuts for the second time among the Step II I that silicon single crystal or polysilicon are carried out line cutting for the third time.
The cutting process of line for the third time described in the line cutting second time described in the line cutting first time described in the step I, the Step II I and the step IV, all adopt multi-line cutting machine and routinely wire cutting technology cut.
Embodiment 1
In the present embodiment, during the preparation additive: taking by weighing molecular weight is polyoxyethylene glycol (PEG200) 9.65kg of 200D (200 dalton), permeate agent is secondary alkyl ethoxylated (JFC) 0.1kg of polyoxyethylene, ether alcohol class promoting agent is AEO-7 nonionogenic tenside 0.1kg, anti-extreme pressure sequestrant is fatty alcohol sulfate monoethanolamine salt (ASEA) 0.05kg, and washing assistant is polyvinylpyrrolidone (PVP-k25) 0.1kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 35 ℃ the polyoxyethylene glycol (PEG200), stirs 5 minutes to evenly, the 10kg additive.
During the preparation additive, select the suitable polyoxyethylene glycol of molecular weight earlier as solvent.At first wire cutting liquid itself is a principal constituent with the polyoxyethylene glycol exactly, and secondly other all components has solvability preferably again in polyoxyethylene glycol.Permeate agent has the effect of lubricant concurrently, can greatly reduce the surface tension of mortar liquid component, make mortar be easy to be penetrated between solid particulate and the silicon chip, has the rubbing effect that reduces between abrasive material, smear metal and the silicon chip surface, reduce physical abuse effectively, and can give full play to the cooling effect of liquid, prevent the accumulation of silicon chip surface thermal stresses.Ether alcohol class promoting agent is a tween, has the lubrication of enhance liquid, makes active agent molecule be adsorbed in silicon chip surface, and can stop solid particulate to deposit again, helps the cleaning of silicon chip.Anti-extreme pressure sequestrant is organophosphate or the sulfuric ester with 10 above polyoxyethylene segments, non-metallic ion and contain hydramine segmental sequestrant: it can form stable chelate to metal ion on the one hand for it, has the performance of good removal metal ion; Simultaneously, anti-effectively extreme pressure friction reducing effect has also been played in the existence of phosphoric acid ester or sulfuric ester polar group, reduces the steel wire wearing and tearing and can improve cutting effect simultaneously.Washing assistant is a polyvinylpyrrolidone, has anti-soil dirt redeposition performance, the follow-up cleaning performance of silicon chip is had preferably improve, and polyvinylpyrrolidone also has certain complex performance simultaneously.
When obtained additive is used, the wire cutting liquid that is adopted for conventional uses with wire cutting liquid (specifically be cutting liquid that Liaoning AoKe Chemical Co., Ltd produce) and the silicon carbide (1500 of polyoxyethylene glycol as principal constituent
#) abrasive material fully mixes the wire cutting liquid that makes according to 1: 0.95 weight ratio, and employing multiple tracks wire cutting machine (MBS 1000) is with solar level silicon single crystal rod dicing (6 cun silicon chips, solar level).Its use is as follows:
Step I, line cutting for the first time and mortar reclaim: the wire cutting liquid that employing prepares in advance carries out the line cutting first time, and in the line cutting process linear cutting mortar is reclaimed, and the linear cutting mortar that is reclaimed this moment is the mortar after line cuts for the first time.
Step II, additive are added: the additive that mixed preparing is good joins in the mortar after the line cutting first time of reclaiming among the step I with 1: 100 weight ratio under the continuously stirring state, and stir and churning time is 60 minutes, make the linear cutting mortar that is added with additive.
Step II I, line cutting for the second time: adopt the linear cutting mortar that is added with additive described in the Step II that silicon single crystal or polysilicon are carried out the line cutting second time.
Step IV, line cutting for the third time: adopt the mortar after line cuts for the second time among the Step II I that silicon single crystal or polysilicon are carried out line cutting for the third time.
The actual result that uses is: promptly useless sheet (cut, the piebald etc.) rate of cutting for the first time is 0.7% (cutting out 5000 altogether) first; The above-mentioned additive of 10kg is added under constantly stirring in the mortar after first line cutting of the online recovery of 1000kg, fully stirred 60 minutes, can carry out second time behind the stirring and evenly mixing and cut, and needn't add additive again when cutting for the third time.The useless sheet rate of cutting for the second time is 1.3% (cutting out 5000 altogether); The useless sheet rate of cutting for the third time is 2.6% (cutting out 5000 altogether).
Embodiment 2
In the present embodiment, during the preparation additive: take by weighing the polyoxyethylene glycol that molecular weight is 400D (PEG) 9.2kg earlier, permeate agent is secondary alkyl ethoxylated (JFC) 0.1kg of polyoxyethylene, ether alcohol class promoting agent is AEO-12 nonionogenic tenside 0.5kg, anti-extreme pressure sequestrant is alcohol ether phosphate monoester ethanolamine salt 0.1kg, and washing assistant is polyvinylpyrrolidone (PVP-k25) 0.1kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 65 ℃ the polyoxyethylene glycol (PEG), stirs 5 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 90 minutes, and all the other using method are all identical with embodiment 1 with step.It uses the result to be: useless sheet (cut, the piebald etc.) rate of cutting for the first time is 0.74% (cutting out 5000 altogether); In the mortar after the line cutting first time of the above-mentioned additive of 10kg online recovery of adding 1000kg under constantly stirring, fully stirred 90 minutes, can carry out the cutting second time behind the stirring and evenly mixing, needn't add additive again when cutting for the third time.The useless sheet rate of cutting for the second time is 1.4% (cutting out 5000 altogether); The useless sheet rate of cutting for the third time is 2.5% (cutting out 5000 altogether).
Embodiment 3
In the present embodiment, during the preparation additive: take by weighing the polyoxyethylene glycol that molecular weight is 200D (PEG) 5kg earlier, permeate agent is secondary alkyl ethoxylated (JFC) 1kg of polyoxyethylene, ether alcohol class promoting agent is AEO-7 nonionogenic tenside 2kg, anti-extreme pressure sequestrant is alcohol ether phosphate monoester ethanolamine salt 1kg, and washing assistant is polyvinylpyrrolidone (PVP-k30) 1kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 120 ℃ the polyoxyethylene glycol (PEG), stirs 10 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 120 minutes, and all the other using method are all identical with embodiment 1 with step.It uses the result to be: useless sheet (cut, the piebald etc.) rate of cutting for the first time is 0.4% (cutting out 5000 altogether); In the mortar after the line cutting first time of the above-mentioned additive of 10kg online recovery of adding 1000kg under constantly stirring, fully stirred 120 minutes, can carry out the cutting second time behind the stirring and evenly mixing, needn't add additive again when cutting for the third time.The useless sheet rate of cutting for the second time is 1.2% (cutting out 5000 altogether); The useless sheet rate of cutting for the third time is 2.2% (cutting out 5000 altogether).
Embodiment 4
In the present embodiment, during the preparation additive: take by weighing the polyoxyethylene glycol that molecular weight is 600D (PEG600) 7.3kg earlier, permeate agent is octyl phenol polyoxy ethene (3) ether (JFC) 0.1kg, ether alcohol class promoting agent is AEO-10 nonionogenic tenside 2kg, anti-extreme pressure sequestrant is alcohol ether phosphate monoester ethanolamine salt 0.5kg, and washing assistant is polyvinylpyrrolidone (PVP-k25) 0.1kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 120 ℃ the polyoxyethylene glycol (PEG600), stirs 10 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 90 minutes, and all the other using method are all identical with embodiment 1 with step.It uses the result to be: useless sheet (cut, the piebald etc.) rate of cutting for the first time is 0.62% (cutting out 5000 altogether); In the mortar after the line cutting first time of the above-mentioned additive of 10kg online recovery of adding 1000kg under constantly stirring, fully stirred 90 minutes, can carry out the cutting second time behind the stirring and evenly mixing, needn't add additive again when cutting for the third time.The useless sheet rate of cutting for the second time is 1.4% (cutting out 5000 altogether); The useless sheet rate of cutting for the third time is 2.6% (cutting out 5000 altogether).
Embodiment 5
In the present embodiment, during the preparation additive: take by weighing the polyoxyethylene glycol that molecular weight is 200D (PEG200) 7.2kg earlier, permeate agent is C8-9 alkylphenol-polyethenoxy (7) ether (JFC) 0.5kg, ether alcohol class promoting agent is AEO-10 nonionogenic tenside 1.5kg, anti-extreme pressure sequestrant is alcohol ether phosphate monoester ethanolamine salt 0.5kg, and washing assistant is the mixture 0.3kg of polyvinylpyrrolidone (PVP-k25) and (PVP-k 30); Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 60 ℃ the polyoxyethylene glycol (PEG200), stirs 7 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 120 minutes, and all the other using method are all identical with embodiment 1 with step.It uses the result to be: useless sheet (cut, the piebald etc.) rate of cutting for the first time is 1% (cutting out 2000 altogether); In the mortar after the line cutting first time of the above-mentioned additive of 10kg online recovery of adding 1000kg under constantly stirring, fully stirred 120 minutes, can carry out the cutting second time behind the stirring and evenly mixing, needn't add additive again when cutting for the third time.The useless sheet rate of cutting for the second time is 1.4% (cutting out 2000 altogether); The useless sheet rate of cutting for the third time is 2.4% (cutting out 2000 altogether).
Embodiment 6
In the present embodiment, during the preparation additive: take by weighing the polyoxyethylene glycol that molecular weight is 200D (PEG200) 6.5kg earlier, permeate agent is C8-9 alkylphenol-polyethenoxy (7) ether (JFC) 0.7kg, ether alcohol class promoting agent is the mixture 1.5kg of AEO-7 nonionogenic tenside and AEO-10 nonionogenic tenside, anti-extreme pressure sequestrant is alcohol ether phosphate monoester ethanolamine salt 0.6kg, and washing assistant is polyvinylpyrrolidone (PVP-k25) 0.7kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 50 ℃ the polyoxyethylene glycol (PEG 200), stirs 6 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 100 minutes, and the weight ratio of the mortar after described additive and the line cutting for the first time is 1: 110, and all the other using method are all identical with embodiment 1 with step.
Embodiment 7
In the present embodiment, during the preparation additive: take by weighing the polyoxyethylene glycol that molecular weight is 200D (PEG) 8.2kg earlier, permeate agent is secondary alkyl ethoxylated (JFC) 0.3kg of polyoxyethylene, ether alcohol class promoting agent is AEO-7 nonionogenic tenside 0.8kg, anti-extreme pressure sequestrant is alcohol ether phosphate monoester ethanolamine salt 0.3kg, and washing assistant is polyvinylpyrrolidone (PVP-k30) 0.4kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 100 ℃ the polyoxyethylene glycol (PEG), stirs 8 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 80 minutes, and the weight ratio of the mortar after described additive and the line cutting for the first time is 1: 90, and all the other using method are all identical with embodiment 1 with step.
Embodiment 8
In the present embodiment, during the preparation additive: taking by weighing molecular weight is polyoxyethylene glycol (PEG200) 5.8kg of 200D (200 dalton), permeate agent is secondary alkyl ethoxylated (JFC) 0.8kg of polyoxyethylene, ether alcohol class promoting agent is AEO-7 nonionogenic tenside 1.8kg, anti-extreme pressure sequestrant is fatty alcohol sulfate monoethanolamine salt (ASEA) 0.8kg, and washing assistant is polyvinylpyrrolidone (PVP-k25) 0.8kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 40 ℃ the polyoxyethylene glycol (PEG 200), stirs 9 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 110 minutes, and the weight ratio of the mortar after described additive and the line cutting for the first time is 1: 95, and all the other using method are all identical with embodiment 1 with step.
Embodiment 9
In the present embodiment, during the preparation additive: taking by weighing molecular weight is polyoxyethylene glycol (PEG200) 9.2kg of 200D (200 dalton), permeate agent is secondary alkyl ethoxylated (JFC) 0.2kg of polyoxyethylene, ether alcohol class promoting agent is fatty alcohol polyoxyethylene ether sulfate (AES) 0.3kg, anti-extreme pressure sequestrant is fatty alcohol sulfate monoethanolamine salt (ASEA) 0.1kg, and washing assistant is polyvinylpyrrolidone (PVP-k25) 0.2kg; Again permeate agent, ether alcohol class promoting agent, anti-extreme pressure sequestrant and the washing assistant of above-mentioned value added successively in 95 ℃ the polyoxyethylene glycol (PEG200), stirs 10 minutes to evenly, the 10kg additive.
In the present embodiment, when obtained additive is used, its using method is as different from Example 1: the additive that mixed preparing is good joins first time of being reclaimed among the step I in the linear cutting mortar time in the Step II, churning time is 75 minutes, and the weight ratio of the mortar after described additive and the line cutting for the first time is 1: 105, and all the other using method are all identical with embodiment 1 with step.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, everyly any simple modification that above embodiment did, change and equivalent structure changed, all still belong in the protection domain of technical solution of the present invention according to the technology of the present invention essence.
Claims (8)
1. additive that improves silicon wafer linear cutting mortar utilization ratio, it is characterized in that: by 50%～96.5% polyoxyethylene glycol by weight percentage, 1%～10% permeate agent, 1%～20% ether alcohol class tensio-active agent, 0.5%～10% anti-extreme pressure sequestrant and 1%～10% washing assistant uniform mixing form, the molecular weight of described polyoxyethylene glycol is 200D～600D, described permeate agent is the fatty alcohol-polyoxyethylene ether with 5～10 carbon atoms, described anti-extreme pressure sequestrant is fatty alcohol sulfate monoethanolamine salt ASEA or alcohol ether phosphate monoester ethanolamine salt, and described washing assistant is one or both among polyvinylpyrrolidone PVP-k25 and the polyvinylpyrrolidone PVP-k30.
2. according to the additive of the described raising silicon wafer of claim 1 linear cutting mortar utilization ratio, it is characterized in that: described ether alcohol class tensio-active agent is fatty alcohol polyoxyethylene ether sulfate AES.
3. according to the additive of the described raising silicon wafer of claim 1 linear cutting mortar utilization ratio, it is characterized in that: described ether alcohol class tensio-active agent is one or both in AEO-7 nonionogenic tenside and the AEO-12 nonionogenic tenside.
4. method for preparing the additive that improves silicon wafer linear cutting mortar utilization ratio according to claim 1 is characterized in that this method may further comprise the steps:
Step 1, each component weighing: according to weight percent is 50%～96.5%: 1%～10%: 1%～20%: 0.5%～10%: 1%～10% ratio, polyoxyethylene glycol, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant are carried out weighing respectively;
Step 2, mixed preparing: under 35 ℃～120 ℃ temperature condition, after the polyoxyethylene glycol of institute's weighing in the step 1, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant mixed and fully stirring 5 minutes～10 minutes, make additive.
5. according to the preparation method of the additive of the described raising silicon wafer of claim 4 linear cutting mortar utilization ratio, it is characterized in that: described in the step 2 under 35 ℃～120 ℃ temperature condition, during with the polyoxyethylene glycol of institute's weighing in the step 1, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant uniform mixing, after by heating installation polyoxyethylene glycol being heated to 35 ℃～120 ℃ earlier, permeate agent, ether alcohol class tensio-active agent, anti-extreme pressure sequestrant and washing assistant being added in the polyoxyethylene glycol mix again.
6. method that the additive that improves silicon wafer linear cutting mortar utilization ratio is according to claim 1 used is characterized in that this method may further comprise the steps:
Step I, line cutting for the first time and mortar reclaim: adopt the wire cutting liquid for preparing in advance that silicon single crystal or polysilicon are carried out the line cutting first time, and in the line cutting process linear cutting mortar is reclaimed, the linear cutting mortar that is reclaimed this moment is the mortar after line cuts for the first time; Described wire cutting liquid for conventional uses cut liquid with polyoxyethylene glycol as the silicon single crystal cutting liquid or the polysilicon of principal constituent;
Step II, additive are added: the additive that mixed preparing is good joins in the mortar after the line cutting first time of reclaiming among the step I with 1: 100 ± 10 weight ratio under the continuously stirring state, and stir, make the linear cutting mortar that is added with additive;
Step II I, line cutting for the second time: adopt the linear cutting mortar that is added with additive described in the Step II that silicon single crystal or polysilicon are carried out the line cutting second time;
Step IV, line cutting for the third time: adopt the mortar after line cuts for the second time among the Step II I that silicon single crystal or polysilicon are carried out line cutting for the third time;
The cutting process of line for the third time described in the line cutting second time described in the line cutting first time described in the step I, the Step II I and the step IV, all adopt multi-line cutting machine and routinely wire cutting technology cut.
7. according to the using method of the additive of the described raising silicon wafer of claim 6 linear cutting mortar utilization ratio, it is characterized in that: when fully stirring in the Step II, churning time is 60 minutes～120 minutes.
8. according to the using method of the additive of claim 6 or 7 described raising silicon wafer linear cutting mortar utilization ratios, it is characterized in that: when the additive that mixed preparing is good joined in the mortar after the line cutting first time of reclaiming among the step I under the continuously stirring state in the Step II, described additive was 1: 100 with the weight ratio of the back of line cutting for the first time mortar.
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| US11015104B2 (en) | 2017-02-03 | 2021-05-25 | Saudi Arabian Oil Company | Cement slurries, cured cements and methods of making and use thereof |
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| CN102827672A (en) * | 2011-06-17 | 2012-12-19 | 比亚迪股份有限公司 | Cutting liquid and preparation method thereof |
| CN103395132B (en) * | 2013-08-02 | 2015-04-08 | 英利集团有限公司 | Method for adjusting and detecting utilization proportion of old mortar in silicon wafer cutting |
| CN106010760A (en) * | 2016-05-19 | 2016-10-12 | 常州向鼎新材料科技有限公司 | Mortar additive for solar slicing as well as preparation method and use method thereof |
| CN106047464A (en) * | 2016-06-29 | 2016-10-26 | 无锡伊佩克科技有限公司 | Preparation method of water-based micro-emulsification cutting fluid |
| CN106635321A (en) * | 2016-11-14 | 2017-05-10 | 武汉宜田科技发展有限公司 | Mortar additive for mortar wire cutting single crystal / polycrystalline silicon wafer |
| CN114179238A (en) * | 2021-12-07 | 2022-03-15 | 中环领先半导体材料有限公司 | Research and development method for large-size semiconductor diamond wire fine wire cutting technology |
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| CN101823712A (en) * | 2010-04-02 | 2010-09-08 | 河南新大新材料股份有限公司 | Recovery processing method of silicon slice cut waste mortar |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823712A (en) * | 2010-04-02 | 2010-09-08 | 河南新大新材料股份有限公司 | Recovery processing method of silicon slice cut waste mortar |
| CN101928630A (en) * | 2010-05-19 | 2010-12-29 | 兰溪市德圣龙电子材料有限公司 | Preparation method for solar silicon wafer linear cutting mortar |
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| US11015104B2 (en) | 2017-02-03 | 2021-05-25 | Saudi Arabian Oil Company | Cement slurries, cured cements and methods of making and use thereof |
| US11015105B2 (en) | 2017-02-03 | 2021-05-25 | Saudi Arabian Oil Company | Cement slurries, cured cements and methods of making and use thereof |
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