CN201046385Y - Apparatus for diluting chemical stock solution - Google Patents

Apparatus for diluting chemical stock solution Download PDF

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Publication number
CN201046385Y
CN201046385Y CNU200620138337XU CN200620138337U CN201046385Y CN 201046385 Y CN201046385 Y CN 201046385Y CN U200620138337X U CNU200620138337X U CN U200620138337XU CN 200620138337 U CN200620138337 U CN 200620138337U CN 201046385 Y CN201046385 Y CN 201046385Y
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CN
China
Prior art keywords
concentration
liquid measure
former liquid
water
dilution
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Expired - Fee Related
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CNU200620138337XU
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Chinese (zh)
Inventor
陈厚名
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CHONGYUE SCIENCE AND TECHNOLOGY Co Ltd
Topco Scientific Co Ltd
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CHONGYUE SCIENCE AND TECHNOLOGY Co Ltd
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Priority to CNU200620138337XU priority Critical patent/CN201046385Y/en
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Abstract

The utility model relates to a device used for preparing aiming concentration mixed solution; the mixed solution is prepared by diluting acid or alkali chemicals raw liquor utilizing pure water. The technical proposal of the utility model is that: excessive aiming concentration raw liquor and quantity of water are used for diluting, the potential titration method is used for analyzing the concentration deviation between the diluted solution and the aiming solution, and for computing the deficit amount of effluent, then, 100% quantity of deficit water is added in the diluted solution to reach the aiming concentration; then, the potential titration method is used again for analyzing the concentration deviation between the diluted solution and the aiming solution, and for computing the deficit amount of effluent, then, 100% quantity of deficit water is added in the diluted solution to reach the aiming concentration.

Description

Device with the former liquid measure dilution of chemicals
Technical field:
The utility model is about a kind of method of the former liquid measure dilution with chemicals such as acid or alkali and is used for the equipment of this dilution.More detailed it, the utility model is about a kind of method that the former liquid measure of chemicals such as acid or alkali is diluted, when for example diluting the alkaline developer that positive photoresistance uses with pure water, it can reach the diluted concentration of being desired with the higher degree of accuracy and efficient, and about a kind of equipment that is used to carry out this dilution process.
Background technology
When making precision component such as semiconductor element, use a kind of alkali lye with strict control concentration.For example, use the solution of alkaline developer such as tetramethylammonium hydroxide (TMAH) to be used as the developer of positive photoresistance, the concentration that needs to adjust this developer make the tolerance with respect to aimed concn (for example 2.38 weight %) be generally+-0.001 weight % in.Note that the tolerance here only is an example.
Traditionally, general practice is to transport the developer of adjusting to aimed concn by developer manufacturer to give the field of employment.Yet this practice needs high shipment and delivery cost when implementing, and therefore transports the former liquid measure of developer recently after deliberation and dilutes former liquid measure in the field of employment with pure water.So (field of employment) is with the method and apparatus of former liquid measure dilution with the developer of preparation aimed concn after deliberation at the scene.
For example, known techniques is to propose the former liquid measure diluent facilities of a kind of developer, wherein the former liquid measure of alkaline developer and pure water are delivered to a pure water groove with mixing arrangement, and the mixed solution that is taken out a part by tank diameter is controlled this former liquid measure of delivering to mixing arrangement and the flow velocity of pure water simultaneously to measure the electrical conductivity of solution.The advantage of this diluent facilities is for can be fast and mat electrical conductivity method (electrode method) is analyzed mixed solution in time concentration.
Yet the dilution technology of this use electrical conductivity method has the accuracy of measurement and the problem of stability, as being easy to produce measure error because of the variations in temperature of electrode, or amplify this measure error because of the variation of the pollution of electrode surface or electrode performance, therefore limited according to this accuracy of commonly using the prepared developer of dilution technology.Therefore, expected to develop a kind of equipment, it can show the developer of former liquid measure and preparation aimed concn with higher accuracy and efficient with the pure water dilution.
Because this case creator is for the result of subject research, have been found that when mat dilutes former liquid measure and prepares alkaline developer, though energy mat potentiometric titration can be come the concentration of analytical solution with higher accuracy, but titration consumes quite long analysis time, and itself can not be applied to the continuous control of the flow velocity of the former liquid measure of being supplied and pure water immediately.Moreover, this case creator studies in earnest according to the resulting knowledge of above-mentioned discovery so that the advantage of optimum utilization titration, and is that mat merges that this potentiometric titration is mixed with the particular processing method and when handling the former liquid measure of chemicals such as acid or alkali and pure water. can take mixed solution to aimed concn (target concentration) in higher accuracy of short time.
The utility model content:
The purpose of this utility model is to provide a kind of device that the former liquid measure of chemicals such as acid or alkali is diluted, and it can reach the concentration dilution of being desired with the higher degree of accuracy and efficient.
For reaching above-mentioned purpose, the utility model utilizes and a kind ofly with pure water the former liquid measure dilution of chemicals such as acid or alkali is given on the device of the present utility model with the method for the mixed solution for preparing a kind of aimed concn, and its method step comprises:
(1) dilute with the excessive stoste of aimed concn and the water of capacity, dilution adds the water of 100% deficiency, to reach the concentration that target is diluted again after after understanding its concentration and aimed concn difference by the potentiometric titration analysis, calculate the deficiency amount of water outlet.
(2) after the dilution, continuous understand its concentration and aimed concn difference via the potentiometric titration analysis after, calculate the deficiency amount of water outlet or stoste, add the water or the former liquid measure of 100% deficiency again, to reach the concentration that target is diluted.
According to the said method step, a kind of device that the former liquid measure of chemicals such as acid or alkali is diluted provided by the utility model can include:
One stoste measuring tank is stored former liquid measure in it;
One preparation vessel wherein mixes former liquid measure and pure water to prepare a kind of mixed solution of aimed concn;
One former liquid measure feed system uses that former liquid measure is supplied to this preparation vessel by this stoste measuring tank;
One pure water feed system uses that pure water is supplied to this preparation vessel;
One uses the concentration measurement system of potentiometric titration, uses the concentration of measuring the mixed solution in this preparation vessel;
One control system, controlling the operation of those elements and having function is that the concentration measurement of the mixed solution in this preparation vessel and the thresholding of goal-selling concentration are made comparisons, earlier that aimed concn is the excessive stoste and the water of capacity dilute, dilution is after after understanding its concentration and aimed concn difference by the potentiometric titration analysis, calculate the deficiency amount of water outlet, the water that adds 100% deficiency again, to reach the concentration of target dilution, dilute follow-up understand its concentration and aimed concn difference via the potentiometric titration analysis again after, calculate the deficiency amount of water outlet or stoste, add the water or the former liquid measure of 100% deficiency again, deliver to this preparation vessel.
The beneficial effects of the utility model are: a kind of device that the former liquid measure of chemicals such as acid or alkali is diluted that provides, can reach needed concentration dilution with the higher degree of accuracy and efficient.
Description of drawings:
Fig. 1 is with the diluted concentration and the corresponding time diagram of the device of the former liquid measure dilution of chemicals such as acid or alkali in the utility model;
Fig. 2 is the device schematic diagram that in the utility model the former liquid measure of chemicals such as acid or alkali is diluted
The figure number explanation:
1: high standard concentration; 2: aimed concn;
3: low mark concentration; 4: water;
5: stoste; 6: the target dilution;
7: potentiometric titrimeter.
The specific embodiment:
Followingly the utility model one preferred embodiment is described with reference to accompanying drawing.Among this embodiment, narration is diluted the former liquid measure of alkaline developer according to the utility model, but the utility model also can be applicable to dilute the former liquid measure of the chemicals such as bronsted lowry acids and bases bronsted lowry of other kinds, as long as mat suitably changes former liquid measure, titrimetric standard solution, goal-selling concentration and other conditions and can make acid-base titration to these solution.
At first, explain according to dilution principle of the present utility model.Dilution principle of the present utility model be a kind of with pure water with the former liquid measure dilution of alkaline developer method with the developer of preparation aimed concn.Developer prepared in the utility model comprises inorganic base aqueous solution, comprises sodium phosphate, sodium hydroxid, sodium silicate or analog and other inorganic bases; The organic base aqueous solution; Tetramethylammonium hydroxide (TMAH) aqueous solution; Tetramethylphosphonihydroxide hydroxide base monoethanol aqueous ammonium or the like.As the former liquid measure that the utility model institute desire is handled, for example use above-mentioned solution wherein the concentration of this composition set into about 10 to 30 percentage by weights.As the pure water of dilution usefulness, use the so-called ultra-pure water that desalt is obtained with ion exchange resin or other special devices.
The utility model is according to following principle with the device of the former liquid measure dilution of chemicals such as acid or alkali, so that the concentration of the developer of initial preparation is progressively taken to more near aimed concn.This dilution principle comprises:
(1) dilute with the excessive stoste of aimed concn and the water of capacity, dilution adds the water of 100% deficiency, to reach the concentration that target is diluted again after after understanding its concentration and aimed concn difference by the potentiometric titration analysis, calculate the deficiency amount of water outlet.
(2) continue after the above-mentioned dilution, continuous understand its concentration and aimed concn difference via the potentiometric titration analysis after, calculate the deficiency amount of water outlet or stoste, add the water or the former liquid measure of 100% deficiency again, to reach the concentration that target is diluted.
Before carrying out above-mentioned steps, set the upper limit of the aimed concn of prepared developer and acceptable concentration of developer to the scope of lower limit the thresholding of aimed concn (below be called).For example, comprise in the situation of developer of TMAH and water one, the concentration of TMAH is set at 2.380 percentage by weights, and the thresholding of aimed concn is the 2.380+-0.003 percentage by weight.
Please refer to Fig. 1 in the utility model with the diluted concentration and the corresponding time diagram of the device of the former liquid measure dilution of chemicals such as acid or alkali.In Fig. 1, stoste and water are diluted with the excessive stoste of aimed concn and the water of capacity, produce the concentration that surpasses low mark concentration 3 and high standard concentration 1.Afterwards, continuous understand its concentration and aimed concn difference via the potentiometric titration analysis after, the deficiency amount of calculating water outlet or stoste adds the water or the former liquid measure of 100% deficiency, again with the into aimed concn 2 that progressively becomes.
Please refer to the schematic diagram that Fig. 2 operates for the device that in the utility model the former liquid measure of chemicals such as acid or alkali is diluted.In Fig. 2, as above-mentioned shown in Figure 1, dilute with the excessive stoste 5 of aimed concn and the water 4 of capacity, dilution is after after the concentration and aimed concn difference by potentiometric titrimeter 7 understanding target dilutions 6, calculate the deficiency amount of water outlet 4, the water 4 that adds 100% deficiency again, to reach the concentration of target dilution 6, dilute follow-up after the concentration and aimed concn difference of target dilution 6 is understood in the method analysis again via potentiometric titrimeter 7, calculate the deficiency amount of water outlet 4 or stoste 5, the water 4 or stoste 5 amounts that add 100% deficiency again are so that the concentration of target dilution 6 reaches required target diluted concentration.
In the utility model, will sneak in the developer, in order to do by the convergence aimed concn gradually downwards of the value more than the threshold value based on the pure water amount of calculating deficiency 100%.In this kind situation, need two groups of accurate constant-delivery pumps, one group of charging that is used to regulate former liquid measure, and another group is used for pure water, this is disadvantageous with regard to the manufacturing cost of equipment.If the pure water that a kind of method is wherein added is when being in excess in the deficiency of calculating a little, only former liquid measure needs constant-delivery pump or weighing or flow agent accurately to measure, and does not need accurately to measure pure water.
According to dilution principle of the present utility model, the mat potentiometric titration can accurately be measured concentration, supply the deficiency of former liquid measure or pure water, and, very reach the target dilution near the value of aimed concn and with very high accuracy in order to do progressively making concentration of developer concentrate on one with minimum number of steps with specified amount mixing this former liquid measure or pure water less than deficiency.Can utilize following device of the present utility model to implement mentioned above principle effectively.
At first, explain that one is used to dilute the embodiment of the utility model diluent facilities of alkaline developer, but mat suitably changes former liquid measure, titrimetric standard solution, goal-selling concentration and other conditions, and diluent facilities of the present utility model can be used for dilute acid and aqueous slkali.
Diluent facilities of the present utility model is a kind of device that dilutes the former liquid measure of alkaline developer with the developer of preparation aimed concn with pure water.As shown in Figures 1 and 2, this device comprises a stoste measuring tank 5, stores the former liquid measure of developer that will handle, a preparation vessel 6 in it, wherein mat mixes former liquid measure and pure water with the preparation developer, one former liquid measure feed system is used and is sent the system preparation vessel 6, one concentration measurement systems 7 by stoste measuring tank 5 former liquid measure, utilize the constant-current titration technology, use the concentration of developer of measuring in the preparation vessel 6, and a control system (not in diagram), it controls the operation of this element.
Stoste measuring tank 5 is a kind of dashpots, is used to supply former liquid measure and gives preparation vessel 6 when needs, and comprise that one has about 100 to 2, the 000 liters corrosion protection container of internal volume.Stoste measuring tank 5 is furnished with a pipe, and it can connect the carrier container (not in diagram) of bringing in-house former liquid measure into.The former liquid measure that is transferred out by carrier container under the pressure of inert gas is to send in the groove 5 via pipe.Stoste measuring tank 5 can be provided with a nitrogen tube sealing to avoid contacting the air of atmosphere.
Preparation vessel 6 is to be designed for former liquid measure is diluted with the preparation developer, and comprises that one has about 500 to 3, the 000 liters corrosion protection container of internal volume.Preparation vessel 6 is provided with a liquid level gauge 7, and it can be by optics or electrical conductivity type point measurement to measure the former liquid measure or the pure water amount of being supplied.Preparation vessel 6 also can be provided with a nitrogen tube sealing, to avoid ingress of air.
Former liquid measure feed system comprises, a pipe is connected to groove 5 so that take out former liquid measure by it; Pump is used for former liquid measure is delivered to groove 5; One pipe is connected to the outlet side of pump; One switch valve, it controls the supply of former liquid measure to groove 5; And a pipe, be used as the inlet of former liquid measure to groove 5.Pump respectively is a kind of constant-delivery pump, can be with the rotary pump of pressurized state supply liquid storage under the flow velocity of constant and control as one.Two pumps are side by side synthetic and have different discharge capacities so that strengthen the feeding control accuracy according to feed rate.
The pure water feed system comprises; One pure water supply pipe; Pair of switches valve and be used to control the supply of pure water to groove 4; And a pipe, serve as the inlet of pure water to groove 4.Pipe is to be connected to a relevant pure water manufacturing equipment, utilizes ion exchange resin or other devices that pure water further is evolved into ultra-pure water in this equipment, and under the pressure of set pump prepared ultra-pure water is sent by the mat pure water manufacturing equipment.This switch valve is side by side configuration so that strengthen the feeding control accuracy according to the water inlet speed of pure water.
Densimeter 7 is the measurement mechanisms that utilize the constant-current titration technology, for example, and processing procedure titration kit (Dia instrument company system).Concentration measurement system is provided in a side of in the developer circulation and exhaust system that cooperates with groove 6.More detailed it, this concentration measurement system is to be configured in a branch line through the pipe of switch valve.The pure water supply pipe that cleaning titration box is used (not in diagram) is to be connected to concentration measurement system.
Circulation and exhaust system constitute that a pipeline is used to circulate and mixing channel 6 in former liquid measure of developer and pure water and the storage tank (not in illustrating) of prepared developer being delivered to it.In this circulation and exhaust system, the circulatory system comprises: a pipe is connected to groove 6 so that take out developer by it; One pump is supplied with developer down in pressure; One pipe, be connected to the outlet side of pump: a switch valve is used to control the backflow of developer to groove 6; And a pipe, serve as the return duct of doing to groove 6.Exhaust system comprises: a switch valve, be located in the branch line of pipe, and be used for the taking-up of the preparation developer of control flume 6; And a pipe, be used for this developer is directed to storage tank (not in diagram).
Pump in circulation and the exhaust system is that a kind of developer circulation time of working as can guarantee that developer has preferable cycle rate person, and also can take out and transmit prepared developer.This pump is to be located between the pipe.
According in the dilution system of the present utility model, also be provided with a mechanism in the convection current or the stirring of preparation vessel 6, more strengthen the agitating function of groove 6 when following developer with box lunch circulation and exhaust system.This mechanism comprises that one is configured in pipe nozzle (not in diagram) foremost, promptly be at the pipe and the contact place of groove 6, this nozzle is used for being made to enter in the groove 6 so that mat sprays energy by the fluid (developer) that tube end ejects pressurization giving developer physical impact in the groove 6.
In air mix facilities of the present utility model, a kind of control system more is provided, it has specific function and comprises the developer that dilutes and prepare a kind of aimed concn with pinpoint accuracy and efficient in groove 6.This control system (though not in diagram) comprising: a kind of input unit, and the signal of using element such as liquid level gauge, pump, concentration measurement system etc. converts the numerical digit signal to; The operational processes device as the formula controller, comprises micro computer and PC; And an output device, the control signal of using Operation Processor converts anaiog signal to.
In the operation of control module, the concentration of the groove 6 interior developers that the mat concentration measurement system is measured is to make comparisons with the default thresholding of aimed concn, when concentration measurement and thresholding are inconsistent, then calculate the deficiency of the former liquid measure of developer, reach former liquid measure feed system of startup or pure water feed system and give groove 6 with former liquid measure or the pure water of supplying based on deficiency 100% according to measuring concentration and goal-selling concentration.
The above only is an illustrative, but not is restricted person.Anyly do not break away from spirit of the present utility model and category, and, all should be contained in the interest field of the present utility model its equivalent modifications of carrying out or change.

Claims (2)

1. the device with the former liquid measure dilution of chemicals is to utilize pure water that the former liquid measure of chemicals such as acid or alkali is diluted to prepare the device of a mixed solution, it is characterized in that this device comprises:
One stoste measuring tank is stored former liquid measure in it;
One preparation vessel wherein mixes former liquid measure and water to prepare a mixed solution;
One former liquid measure feed system is supplied to this preparation vessel with former liquid measure by this stoste measuring tank;
One water supply system is supplied to this preparation vessel with this water;
One concentration measurement system is measured the concentration of the mixed solution in this preparation vessel;
One control system, control the operation of those elements, the concentration measurement and a goal-selling concentration of mixed solution are made comparisons, after this water of adding capacity is done dilution earlier, after measuring its concentration and this aimed concn difference via concentration measurement system, this water that adds the deficiency amount again is to this preparation vessel.
2. the device with the former liquid measure dilution of chemicals as claimed in claim 1 is characterized in that, this concentration measurement system is more comprised the concentration that a potentiometric titrimeter is measured this mixed solution.
CNU200620138337XU 2006-09-22 2006-09-22 Apparatus for diluting chemical stock solution Expired - Fee Related CN201046385Y (en)

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Application Number Priority Date Filing Date Title
CNU200620138337XU CN201046385Y (en) 2006-09-22 2006-09-22 Apparatus for diluting chemical stock solution

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Application Number Priority Date Filing Date Title
CNU200620138337XU CN201046385Y (en) 2006-09-22 2006-09-22 Apparatus for diluting chemical stock solution

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CN201046385Y true CN201046385Y (en) 2008-04-16

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104483177A (en) * 2014-12-31 2015-04-01 力合科技(湖南)股份有限公司 Automatic water-quality sampling control method and system
CN106179053A (en) * 2016-07-20 2016-12-07 皖西学院 A kind of solution mixing titration appratus
CN110187722A (en) * 2019-05-20 2019-08-30 南京感控通化工产品经营部 The control method and injecting systems of a kind of drug dose calibrating installation, the device

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104483177A (en) * 2014-12-31 2015-04-01 力合科技(湖南)股份有限公司 Automatic water-quality sampling control method and system
CN104483177B (en) * 2014-12-31 2017-09-19 力合科技(湖南)股份有限公司 Water quality automatic sample control method and system
CN106179053A (en) * 2016-07-20 2016-12-07 皖西学院 A kind of solution mixing titration appratus
CN106179053B (en) * 2016-07-20 2018-08-28 皖西学院 A kind of solution mixing titration outfit
CN110187722A (en) * 2019-05-20 2019-08-30 南京感控通化工产品经营部 The control method and injecting systems of a kind of drug dose calibrating installation, the device
CN110187722B (en) * 2019-05-20 2023-02-17 南京巨鲨显示科技有限公司 Drug dose calibration device, control method of drug dose calibration device and injection system

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GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20080416

Termination date: 20091022